CN109402556A - A kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon - Google Patents
A kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon Download PDFInfo
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- CN109402556A CN109402556A CN201811569641.3A CN201811569641A CN109402556A CN 109402556 A CN109402556 A CN 109402556A CN 201811569641 A CN201811569641 A CN 201811569641A CN 109402556 A CN109402556 A CN 109402556A
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- ndfeb magnet
- neodymium iron
- iron boron
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- surfacecti proteon
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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
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- 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
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C14/34—Sputtering
- C23C14/46—Sputtering by ion beam produced by an external ion source
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of physical gas-phase deposite methods of neodymium iron boron surfacecti proteon, include the following steps: S100, carry out chamfer grinding processing to NdFeB magnet, carry out ultrasonic cleaning, drying afterwards；S200, the NdFeB magnet after cleaning, drying is put into vacuum chamber and is heated, be passed through argon gas and hydrogen, then turn on ion source ionization argon gas ion, while the back bias voltage to the load of NdFeB magnet not less than 500 volts carries out ion etching to NdFeB magnet；S300, it carries out NdFeB magnet surface film forming under ion source assisted: continuing to be passed through argon gas protector to working vacuum degree 1 × 10‑1Pa opens ion source and shielding power supply, and aluminium target is loaded 500 volts of pressurizations, bombards NdFeB magnet surface under not less than 150 volts back bias voltages.S400, progress NdFeB magnet post-processing effectively eliminate the growth of column crystal it is hereby achieved that enough kinetic energy gets rid of the limitation of column crystal wall, the generation of gap and pin hole are avoided, to form the good compact metal aluminized coating of anticorrosion ability.
Description
Technical field
The present invention relates to material surface modifying technology field in low temperature plasma physics and chemistry, specially a kind of neodymium iron
The physical gas-phase deposite method of boron surface protection.
Background technique
As current strongest magnetic property material, the application of neodymium iron boron (NdFeB) permanent-magnet material and development are in recent years very
Rapidly, medical treatment, mechanical, automobile, the numerous areas such as electronic device are had been widely used for, and application prospect is very wide；NdFeB
It is made of the rich Nd and richness B and base phase Nd2Fe14B of thin layer phase；Difference mutually contacts with each other, because the difference of electromotive force forms nothing
Number micro cell, thus corrodes, magnet the Nomenclature Composition and Structure of Complexes is caused to change, magnetic property decline.NdFeB chemical property is living
It sprinkles, is easy to corrode under natural environmental condition, seriously hinders its large-scale application, how to obtain high-corrosion resistance
Magnetic material becomes the hot spot of Recent study.
In view of the market prospects and critical role of NdFeB magnet material, external manufacturer all makees the surfacecti proteon of NdFeB
For the important technical links of magnet generation, and there is the following in technology realization in existing NdFeB permanent-magnet material:
(1) NdFeB permanent-magnet material usually works under certain temperature and ambient condition, it is desirable that protects during long-term work
Hold the integrality of its outer dimension and the stability of magnetic performance；When NdFeB material corrodes, surface regional area will be produced
Generation point and structural damage, decline magnetic performance, to influence its practical application；
(2) domestic common plant-scale neodymium iron boron surfacecti proteon processing method is plating and chemical plating at present.Although
These methods can improve the corrosion resisting property of magnet to a certain extent, but itself there is also limitations；Because using these
During method prepares NdFeB protective layer, plating solution may remain in inside NdFeB and hydrogen abstraction reaction may occur for NdFeB,
The yield rate of product is often reduced, and is polluted more serious；Moreover, as newly environmentally friendly draft requires to produce in electronic product for European Union
Middle reduction is found environment friendly and pollution-free new process and is particularly important using plating or chemical plating；In this context, object
Application of the physical vapor deposition technology in Sintered NdFeB anti-corrosion receives more and more extensive concern.
Summary of the invention
In order to overcome the shortcomings of that prior art, the present invention provide a kind of physical vapour deposition (PVD) of neodymium iron boron surfacecti proteon
Method can effectively solve the problem of background technique proposes.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon, includes the following steps:
S100, chamfer grinding processing is carried out to NdFeB magnet, carries out ultrasonic cleaning, drying afterwards；
S200, the NdFeB magnet after cleaning, drying is put into vacuum chamber and is heated, be passed through argon gas and hydrogen, then turn on
Ion source ionization argon gas ion, while the back bias voltage to the load of NdFeB magnet not less than 500 volts carries out ion to NdFeB magnet
Etching.
S300, it carries out NdFeB magnet surface film forming under ion source assisted: continuing to be passed through argon gas protector to work very
Reciprocal of duty cycle 1 × 10-1Pa opens ion source and shielding power supply, and aluminium target is loaded 500 volts and is added under not less than 150 volts back bias voltages
Pressure bombards NdFeB magnet surface.
S400, NdFeB magnet post-processing is carried out.
Further, it to NdFeB magnet chamfering in S100, and is put into vibration mill, it is not small to obtain corner arc
In the NdFeB magnet of 0.5mm, the ultrasonic cleaning, drying of sandblasting and acid-base property solution is then carried out.
Further, the vacuum degree of vacuum chamber is not less than 1 × 10 in S200-2~1Pa, heating NdFeB magnet to 150~
250 DEG C, and after NdFeB magnet reaches temperature range, continuously adding argon gas to working vacuum degree is 3 × 10-3Pa, ion etching
Time be 30min.
Further, S300 intermediate ion source power maintains 4~5 kilowatts, duration 40min.
Further, in s 200, before carrying out NdFeB magnet etching, it is evacuated to 1 × 10-2After pa, it is clear to carry out aura
1h is washed, and then takes out secondary high vacuum to 3 × 10-3Clear target is carried out after pa.
Further, protective gas argon gas can also be passed through in S300 to working vacuum degree 1 × 10-1The load of Pa, NdFeB magnet
150 volts of biass open shielding power supply, and column rafifinal target loads 600 volts of voltages, continue 40min, carry out to NdFeB magnet normal
Advise the film forming of technique.
Further, in the post-processing of S400, Chrome-free or chromic salt is selected to be passivated film as needed
Processing.
Further, it in S100, grinds the NdFeB magnet finished and is placed in supersonic wave cleaning machine and clean, cleaning temperature
It is 50 DEG C, time 5min.
Compared with prior art, the beneficial effects of the present invention are:
The present invention increases the activation energy of magnet surface by the NdFeB magnet surface cleaning in vacuum working environment, and
When NdFeB magnet carries out surface filming, ion source is opened, the unlatching of ion source can greatly increase aluminium atom as aluminium ion
Ionization level, aluminium atom bombardment is big to magnet surface ability, it is hereby achieved that enough kinetic energy gets rid of the limitation of column crystal wall,
The growth for effectively eliminating column crystal, avoids the generation of gap and pin hole, to form the good compact metal aluminium of anticorrosion ability
Coating；
Detailed description of the invention
Fig. 1 is the physical gas-phase deposite method flow chart of neodymium iron boron surfacecti proteon of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 1, the present invention provides a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon, feature exists
In: include the following steps:
S100, chamfer grinding processing is carried out to NdFeB magnet, carries out ultrasonic cleaning, drying afterwards；
S200, the NdFeB magnet after cleaning, drying is put into vacuum chamber and is heated, be passed through argon gas and hydrogen, then turn on
Ion source ionization argon gas ion, while the back bias voltage to the load of NdFeB magnet not less than 500 volts carries out ion to NdFeB magnet
Etching.
S300, it carries out NdFeB magnet surface film forming under ion source assisted: continuing to be passed through argon gas protector to work very
Reciprocal of duty cycle 1 × 10-1Pa opens ion source and shielding power supply, and aluminium target is loaded 500 volts and is added under not less than 150 volts back bias voltages
Pressure bombards NdFeB magnet surface.
S400, NdFeB magnet post-processing is carried out.
Its four-stage specifically includes:
First stage carries out pre-treatment, first chamfering to NdFeB magnet, and ndfeb magnet is placed in vibration mill
In, make the corner arc of magnet not less than 0.5mm, followed by sandblasting, acid-base property solution ultrasonic cleaning is simultaneously dried, to go
Except the greasy dirt rust staining of magnet surface.
Second stage vacuum ionic Bombardment and cleaning is not low to vacuum chamber first to increase magnet surface activation energy
In within the scope of 1 × 10-2~1Pa, while magnet is heated within the scope of 150~250 DEG C, argon gas and hydrogen are passed through in heating process
It prevents magnet from aoxidizing, then passes to protective gas argon gas to 3 × 10-3Pa of working vacuum degree, then open ion source ionization argon gas
It generates argon ion and ion etching is carried out to magnet, while being performed etching to back bias voltage of the magnet load not less than 500 volts, ion is carved
Lose 30min.
Phase III is text message, and available there are two types of technique, the first is common process: being passed through protective gas argon
Gas to 1 × 10-1pa of working vacuum degree, magnet loads 150 volts of biass, opens shielding power supply, and column rafifinal target loads 600 volts
Voltage, aluminium ion are deposited on magnet surface under magnetic fields and form fine and close aluminized coating.Second is ion source assisted work
Skill: protective gas argon gas is passed through to 1 × 10-1 of working vacuum degree, magnet load is not less than 150 volts of back bias voltages, then opens ion
Source, ion source power maintain 4~5 kilowatts, open shielding power supply, and aluminium target loads 500 volts of pressurizations, and the unlatching of ion source can be big
The big aluminium atom that increases becomes aluminum ions ionization level.Two kinds of technique alternatives, duration are 40 minutes.
It further illustrates:
Common process:
Step 1: taking 30 block sizes is 25mm × 25mm × 8mm Sintered NdFeB magnetic patch.
Step 2: above-mentioned first step bulk magnet is placed in vibration mill, the mixed of silicon carbide and Brown Alundum is used
Material carries out chamfering flour milling to it, and silicon carbide and Brown Alundum are 3:2, and compound abrasive weight is 15kg.
Step 3: be first placed in the beaker of dehydrated alcohol for the magnet finished is ground in above-mentioned second step, then to be placed in acetone molten
It in the beaker of liquid, then places the beaker supersonic wave cleaning machine ultrasound and successively cleans, temperature is 50 DEG C, and time 5min has been cleaned
It is dried after finishing.
Step 4: in the magnet shove charge that the cleaning of above-mentioned third step is finished, after closing fire door is evacuated down to 1 × 10-2pa,
It carries out aura to clean 1 hour, carries out clear target after then taking out secondary high vacuum to 3 × 10-3pa, cool down again after clear target.Then start
Plated film.
Step 5: start plated film after the cooling of above-mentioned 4th step, pass first into protective gas argon gas to working vacuum degree 1 ×
10-1pa, magnet load are not less than 150 volts of back bias voltages, then open shielding power supply, and column rafifinal target loads 600 volts of voltages,
Process lasting time 40min, last aluminium ion deposit to form fine and close aluminized coating in magnet surface, through detection institute's film plating layer with a thickness of
6~8 microns.
Step 6: taking ten pieces of progress neutral salt spray tests for appointing in blocky magnet that above-mentioned 4th step plated film finishes, 98 is small
When after observe, there are two pieces of magnet surfaces corrosion rust spots occur.
Ion source assisted technique:
Step 1: taking 30 block sizes is 25mm × 25mm × 8mm Sintered NdFeB magnetic patch.
Step 2: above-mentioned first step bulk magnet is placed in vibration mill, the mixed of silicon carbide and Brown Alundum is used
Material carries out chamfering flour milling to it.
It is placed in the beaker equipped with alcohol and acetone soln step 3: the magnet finished will be ground in above-mentioned second step, then
Supersonic wave cleaning machine ultrasonic cleaning is placed the beaker, is dried after cleaning.
Step 4: in the magnet shove charge that the cleaning of above-mentioned third step is finished, after closing fire door is evacuated down to 1 × 10-2pa,
It carries out aura and cleans 1h, carry out clear target after then taking out secondary high vacuum to 3 × 10-3pa, 30min is performed etching after clear target, then
Cooling.
Step 5: start plated film after the cooling of above-mentioned 4th step, pass first into protective gas argon gas to working vacuum degree 1 ×
10-1pa then opens ion source, and ion source power maintains 4~5 kilowatts, opens shielding power supply, and aluminium target loads 500 volts and adds
Pressure, continues plated film 20min, 5~6 microns of institute's film plating layer thickness using GMIS technique.
Step 6: taking ten pieces of progress neutral salt spray tests for appointing in blocky magnet that above-mentioned 4th step plated film finishes, 200 is small
When after observe, magnet is intact, and surface does not occur corrosion rust spot.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (8)
1. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon, characterized by the following steps:
S100, chamfer grinding processing is carried out to NdFeB magnet, carries out ultrasonic cleaning, drying afterwards；
S200, the NdFeB magnet after cleaning, drying is put into vacuum chamber and is heated, be passed through argon gas and hydrogen, then turn on ion
Source ionization argon gas ion, while the back bias voltage to the load of NdFeB magnet not less than 500 volts carries out ion etching to NdFeB magnet.
S300, it carries out NdFeB magnet surface film forming under ion source assisted: continuing to be passed through argon gas protector to working vacuum degree
1×10-1Pa opens ion source and shielding power supply, and aluminium target is loaded 500 volts of pressurizations under not less than 150 volts back bias voltages, Hong
Hit NdFeB magnet surface.
S400, NdFeB magnet post-processing is carried out.
2. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that: S100
In to NdFeB magnet chamfering, and be put into vibration mill, obtain the NdFeB magnet that corner arc is not less than 0.5mm, with
The ultrasonic cleaning, drying of sandblasting and acid-base property solution is carried out afterwards.
3. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that: S200
The vacuum degree of middle vacuum chamber is not less than 1 × 10-2~1Pa, heating NdFeB magnet reach to 150~250 DEG C, and in NdFeB magnet
After temperature range, continuously adding argon gas to working vacuum degree is 3 × 10-3Pa, the time of ion etching are 30min.
4. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that: S300
Intermediate ion source power maintains 4~5 kilowatts, duration 40min.
5. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that:
In S200, before carrying out NdFeB magnet etching, it is evacuated to 1 × 10-2After pa, carries out aura and clean 1h, and then take out secondary height
Vacuum is to 3 × 10-3Clear target is carried out after pa.
6. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that: S300
In can also be passed through protective gas argon gas to working vacuum degree 1 × 10-1Pa, NdFeB magnet load 150 volts of biass, open sputtering electricity
Source, column rafifinal target load 600 volts of voltages, continue 40min, and the film forming of common process is carried out to NdFeB magnet.
7. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that:
In the post-processing of S400, Chrome-free or chromic salt is selected to be passivated processing to film as needed.
8. a kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon according to claim 1, it is characterised in that:
It in S100, grinds the NdFeB magnet finished and is placed in supersonic wave cleaning machine and clean, cleaning temperature is 50 DEG C, time 5min.
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| CN201811569641.3A CN109402556A (en) | 2018-12-21 | 2018-12-21 | A kind of physical gas-phase deposite method of neodymium iron boron surfacecti proteon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111575664A (en) * | 2020-05-18 | 2020-08-25 | 中国科学院力学研究所 | Film coating method for realizing cold plating on surface of magnetic material by utilizing ionization sputtering technology |
| WO2021083166A1 (en) * | 2019-10-28 | 2021-05-06 | 华南理工大学 | Method for improving coercivity, wear resistance and corrosion resistance properties of neodymium iron boron magnet |
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| CN102002669A (en) * | 2010-12-17 | 2011-04-06 | 河南理工大学 | Method for plating stainless-steel protective coating on surface of sintered NdFeB magnet through magnetron sputtering |
| CN104651782A (en) * | 2013-11-18 | 2015-05-27 | 北京中科三环高技术股份有限公司 | Magnet surface treatment method and sintered neodymium-iron-boron magnet |
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2018
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| CN102002669A (en) * | 2010-12-17 | 2011-04-06 | 河南理工大学 | Method for plating stainless-steel protective coating on surface of sintered NdFeB magnet through magnetron sputtering |
| CN104651782A (en) * | 2013-11-18 | 2015-05-27 | 北京中科三环高技术股份有限公司 | Magnet surface treatment method and sintered neodymium-iron-boron magnet |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021083166A1 (en) * | 2019-10-28 | 2021-05-06 | 华南理工大学 | Method for improving coercivity, wear resistance and corrosion resistance properties of neodymium iron boron magnet |
| CN111575664A (en) * | 2020-05-18 | 2020-08-25 | 中国科学院力学研究所 | Film coating method for realizing cold plating on surface of magnetic material by utilizing ionization sputtering technology |
| CN111575664B (en) * | 2020-05-18 | 2021-08-17 | 中国科学院力学研究所 | Film coating method for realizing cold plating on surface of magnetic material by utilizing ionization sputtering technology |
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Application publication date: 20190301 |