CN110129733A - A kind of Sintered NdFeB magnet and preparation method thereof with composite film - Google Patents
A kind of Sintered NdFeB magnet and preparation method thereof with composite film Download PDFInfo
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- CN110129733A CN110129733A CN201910533157.3A CN201910533157A CN110129733A CN 110129733 A CN110129733 A CN 110129733A CN 201910533157 A CN201910533157 A CN 201910533157A CN 110129733 A CN110129733 A CN 110129733A
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- 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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- 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
- C23C14/0641—Nitrides
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- 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
- C23C14/08—Oxides
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- 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
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
The present invention relates to magnetic material surface protection technique fields more particularly to a kind of Sintered NdFeB magnet surface recombination film layer and preparation method thereof.The Sintered NdFeB magnet with composite film includes magnet body, and is cascadingly set on aluminum membranous layer, aluminum oxide film layer and the titanium nitride film on magnet body surface.Sintered NdFeB magnet provided by the invention, by being sequentially depositing aluminum membranous layer, aluminum oxide film layer and titanium nitride film, it can interrupt and close the structure effect of the tissue defects through film, it avoids to form the tissue defects such as the pin hole through plural layers, micro-crack, improves the corrosion resistance of magnet.Multilayer film alternating deposit reduces film layer internal stress, keeps titanium nitride finer and close, also enhances between film layer and the binding force of film layer and substrate, further enhances corrosion resistance.In addition, also improving the fire-resistant oxidation resistant of magnet by the setting of aluminum oxide film layer, by the deposition of titanium nitride film, the erosion resistance of magnet is improved.
Description
Technical field
The present invention relates to magnetic material surface protection technique field more particularly to a kind of sintering neodymium iron with composite film
Boron magnet and preparation method thereof.
Background technique
With flourishing for science and technology, Sintered NdFeB magnet is in new-energy automobile manufacture, wind power generation, Novel electric
The high-tech industrial application such as machine is very extensive.
Physics phase depositing titanium nitride film process is mostly used to be surface-treated Sintered NdFeB magnet in industry at present,
And generally there are the tissue defects such as pin hole, micro-crack in single titanium nitride membrane, therefore, corrode when in application high humid and warm environment
Medium will be encroached on by the path that above-mentioned tissue defects are formed to Sintered NdFeB magnet, and the resistance to of Sintered NdFeB magnet is caused
Corrosivity is poor, to influence the service performance of Sintered NdFeB magnet.
Summary of the invention
(1) technical problems to be solved
For existing technical problem, the present invention provide a kind of Sintered NdFeB magnet with composite film and its
Preparation method, the corrosion resistance for solving Sintered NdFeB magnet in the prior art is poor, influences making for Sintered NdFeB magnet
The problem of with performance.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
On the one hand, the embodiment of the invention provides a kind of Sintered NdFeB magnets with composite film, including magnet sheet
Body, and it is cascadingly set on aluminum membranous layer, aluminum oxide film layer and the titanium nitride film on the magnet body surface.
According to the present invention, the aluminum membranous layer with a thickness of 0.1~0.7 μm；The aluminum oxide film layer with a thickness of 0.1~
0.7μm；The titanium nitride film with a thickness of 0.4~1.0 μm；
The overall thickness of the composite film is 1.0~2.4 μm.
On the other hand, the embodiment of the invention also provides a kind of preparation sides of Sintered NdFeB magnet with composite film
Method, comprising the following steps:
The magnet body surface is polished, polished and cleaned；
The aluminum membranous layer, the aluminum oxide film layer are sequentially depositing on the magnet body surface using physical vaporous deposition
With the titanium nitride film.
Such as the above method, it is described magnet body surface is polished, polished and is cleaned include:
#400, #600, #1000, #1500, #2000 sand paper is utilized respectively successively to polish the surface of the magnet body；
It is polished using surface of the polishing machine to the magnet body that polishing is completed, until it is in mirror-like；
By polishing complete the magnet body be placed sequentially in dehydrated alcohol and acetone soln carry out ultrasonic cleaning 5~
10min, and clean repeatedly twice；
The vacuum of physical vapor deposition equipment is put into after the magnet body that cleaning terminates is dried
In room, starting vacuum pump is evacuated vacuum chamber, and base vacuum is 1 × 10-3Pa, the flow set of argon gas is 10~
20sccm, operating pressure are set as 0.5~1Pa, by Ar+ glow discharge effect to the further sputter clean of matrix 10~
30min。
It is described to be sequentially depositing the aluminium film on the magnet body surface using physical vaporous deposition such as the above method
Layer, the aluminum oxide film layer and the titanium nitride film include:
Be filled with argon gas to air pressure to 0.4~1.0Pa to the vacuum chamber, open target power supply, adjust target power output to 80~
120W, by magnetron sputtering in the processed magnet body deposition of aluminum film layer；
Being filled with argon gas to air pressure to the vacuum chamber is 0.4~1.0Pa, opens radio-frequency power supply, adjusts radio-frequency power 250W
~400W, by radio-frequency sputtering on the aluminum membranous layer of the magnet body deposited oxide aluminum membranous layer；
The vacuum indoor gas is discharged, according to argon flow 30sccm and nitrogen flow 4sccm by argon gas and nitrogen
Vacuum chamber is filled with until gas pressure in vacuum is 0.4~1.0Pa, to titanium target energization, adjusting titanium target power is 100~150W, in institute
Depositing titanium nitride film layer in the aluminum oxide film layer of magnet body is stated, closes titanium target power supply after the completion.
Such as the above method, the anti-corrosion film layer that deposits on magnet includes:
The pre-sputtering of 10min is carried out before deposition, to target all every time to remove the pollutant of target material surface attachment；
Sample stage baffle is removed, is sequentially depositing aluminium film, pellumina, titanium nitride film on the magnet.
Such as the above method, the purity of the nitrogen is greater than 99.9wt%, and the purity of the argon gas is greater than 99.9wt%.
Such as the above method, the aluminium purity is greater than 99wt%.
Such as the above method, the aluminium oxide purity is greater than 99wt%.
Such as the above method, the titanium purity is greater than 99wt%.
(3) beneficial effect
The beneficial effects of the present invention are:
Sintered NdFeB magnet provided by the invention, by the surface sandwich diaphragm layer structure in magnet ontology, from base
For body material surface to composite film surface, composite film is followed successively by aluminum membranous layer, aluminum oxide film layer and titanium nitride film.The composite membrane
Layer has good hardness and corrosion-resistant protective performance.By magnet body surface be sequentially depositing aluminum membranous layer, aluminum oxide film layer and
Titanium nitride film can interrupt and close the structure effect of the tissue defects through film, run through multilayer so as to avoid being formed
The tissue defects such as pin hole, the micro-crack of film improve the corrosion resistance of Sintered NdFeB magnet.Moreover, because magnet ontology
The composite membrane on surface is formed by multilayer film alternating deposit, reduces film layer internal stress, is kept top layer titanium nitride finer and close, is increased simultaneously
Between strong film layer and the binding force between film layer and matrix, to further enhance corrosion resistance.In addition, passing through oxidation
The setting of aluminum membranous layer and titanium nitride film also improves the fire-resistant oxidation resistant and erosion resistance ability of Sintered NdFeB magnet.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the Sintered NdFeB magnet with composite film provided in an embodiment of the present invention.
[description of symbols]
1: magnet body；2: aluminum membranous layer；3: aluminum oxide film layer；4: titanium nitride film.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
As shown in Figure 1, the embodiment of the invention provides a kind of Sintered NdFeB magnet with composite film, including magnet
Ontology 1, and it is cascadingly set on aluminum membranous layer 2, aluminum oxide film layer 3 and the titanium nitride film 4 on 1 surface of magnet body.
The embodiment of the present invention is cascading aluminum membranous layer 2, aluminum oxide film layer 3 by the surface in Sintered NdFeB magnet
It solves magnet body surface to form composite film on the surface of magnet body with titanium nitride film 4 and single nitridation is set
The defects of pin hole present in titanium film layer, micro-crack, poor heat-resisting quantity, moreover, this kind of multilayered structure additionally aids reduction film
Internal stress between layer；Aluminum membranous layer 2 can be used as the binding force that buffer layer helps to improve aluminium oxide and magnet, and deposited oxide
Magnet fire-resistant oxidation resistant then can be improved in aluminum membranous layer 3, meanwhile, depositing titanium nitride film layer 4 can also further increase film layer
Hardness and corrosion resistance.
Sintered NdFeB magnet provided by the invention, by the surface sandwich diaphragm layer structure in magnet ontology, from base
For body material surface to composite film surface, composite film is followed successively by aluminum membranous layer, aluminum oxide film layer and titanium nitride film.The composite membrane
Layer has good hardness and corrosion-resistant protective performance.By magnet body surface be sequentially depositing aluminum membranous layer, aluminum oxide film layer and
Titanium nitride film can interrupt and close the structure effect of the tissue defects through film, run through multilayer so as to avoid being formed
The tissue defects such as pin hole, the micro-crack of film improve the corrosion resistance of Sintered NdFeB magnet.Moreover, because magnet ontology
The composite membrane on surface is formed by multilayer film alternating deposit, reduces film layer internal stress, is kept top layer titanium nitride finer and close, is increased simultaneously
Between strong film layer and the binding force between film layer and matrix, to further enhance corrosion resistance.In addition, passing through oxidation
The setting of aluminum membranous layer and titanium nitride film also improves the fire-resistant oxidation resistant and erosion resistance ability of Sintered NdFeB magnet.
In an optional embodiment, referring to Fig. 1, this has in the Sintered NdFeB magnet of composite film, aluminum membranous layer 2
Thickness can be 0.1~0.7 μm；The thickness of aluminum oxide film layer 3 can be 0.1~0.7 μm；The thickness of titanium nitride film 4 can be with
It is 0.4~1.0 μm；The overall thickness of composite film can be 1.0~2.4 μm.By carrying out different selections to three thicknesses of layers,
Not only the surface roughness of each film layer can be made smaller, but also can guarantee the hardness requirement of each film layer, while also assuring three
Biggish binding force is all had between magnet body, it is not easy to fall off.It should be noted that in order to guarantee the sintered NdFeB
The hardness and corrosion resistance of magnet, while the thickness of each film layer reaches requirement, the overall thickness of film layer cannot be too small, with
Avoid influencing the corrosion resistance of the Sintered NdFeB magnet.
The embodiment of the invention also provides a kind of preparation methods of Sintered NdFeB magnet with composite film, can wrap
Following steps are included, referring to Fig. 1.
S1: 1 surface of magnet body is polished, polished and is cleaned；
S2: aluminum membranous layer 2, aluminum oxide film layer 3 and nitridation are sequentially depositing on 1 surface of magnet body using physical vaporous deposition
Titanium film layer 4.
In step s1,1 surface of magnet body is polished, polished and cleaned, magnet table can be effectively removed
Impurity on face so that post-depositional composite film can and the stronger combination of magnet body 1, prevent from falling off,
It avoids and participates in impurity in composite film, the corrosion resistance of the composite film is had an impact.
In step s2, physical vaporous deposition depositional coating has film forming even compact, strong etc. with the binding force of matrix
Feature.Specifically, deposition of aluminum film layer 2, so that aluminum membranous layer 2 is used as buffer layer, to improve the binding force of aluminium oxide and magnet, in aluminium
Deposited oxide aluminum membranous layer 3 on film layer 2, the fire-resistant oxidation resistant of magnet then can be improved in aluminum oxide film layer 3, in pellumina
Depositing titanium nitride film layer 4 on layer 3, can be improved film hardness and corrosion resistance.The structure setting of this kind of trilamellar membrane layer, avoids
It is formed through tissue defects such as pin hole, the micro-cracks of plural layers, improves the corrosion resistance of Sintered NdFeB magnet, and
Improve the fire-resistant oxidation resistant of the Sintered NdFeB magnet.
In an optional embodiment, referring to Fig. 1, above-mentioned steps S1 can specifically include following steps:
#400, #600, #1000, #1500, #2000 sand paper is utilized respectively successively to polish the surface of magnet body 1；
It is polished using surface of the polishing machine to the magnet body 1 that polishing is completed, until it is in mirror-like；
By polishing complete magnet body 1 be placed sequentially in dehydrated alcohol and acetone soln carry out ultrasonic cleaning 5~
10min, and clean repeatedly twice；
The vacuum of physical vapor deposition equipment is put into after the magnet body 1 that cleaning terminates is dried
In room, starting vacuum pump is evacuated vacuum chamber, and base vacuum is 1 × 10-3Pa, the flow set of argon gas is 10~
20sccm, operating pressure are set as 0.5~1Pa, by Ar+ glow discharge effect to the further sputter clean of matrix 10~
30min。
Firstly, the sand paper using #400, #600, #1000, #1500, #2000 different model successively carries out magnet surface
Polishing, can effectively remove the larger particles of magnet surface, keep surface more smooth, at the same time it can also remove magnet sheet
The oxidation film on 1 surface of body；Magnet body 1 plus polishing cream that polishing is completed are polished on polishing machine again, with further
The tiny particles content for removing 1 surface of magnet body, so that then 1 surface of magnet body more smooth pieces utilize dehydrated alcohol
It is cleaned by ultrasonic with acetone soln, the impurity that 1 surface of magnet body not easily passs through polishing and polishing removal can be dissolved, made
The cleaning for obtaining 1 surface of magnet body is more thorough, reduces impurity residual, thus avoid influencing the corrosion resistance of composite membrane, finally,
Ar+ glow discharge effect carries out 10~30min of bombardment to 1 surface of magnet body, can be further to 1 surface of magnet body
It is cleaned, removes surface contamination sundries, be ready for deposition composite film.
In an optional embodiment, referring to Fig. 1, above-mentioned steps S2 can specifically include following steps:
Being filled with argon gas to air pressure to vacuum chamber is 0.4~1.0Pa, opens target power supply, adjusts target power output to 80~120W, leads to
Cross magnetron sputtering deposition of aluminum film layer in processed magnet body 1；
To vacuum chamber be filled with argon gas to air pressure be 0.4~1.0Pa, open radio-frequency power supply, adjust radio-frequency power 250W~
400W, by radio-frequency sputtering on the aluminum membranous layer 2 of magnet body 1 deposited oxide aluminum membranous layer 3；
The vacuum indoor gas is discharged, according to argon flow 30sccm and nitrogen flow 4sccm by argon gas and nitrogen
Vacuum chamber is filled with until air pressure is 0.4~1.0Pa, to titanium target energization, adjusting titanium target power is 100~150W, in magnet body 1
Aluminum oxide film layer 3 on depositing titanium nitride film layer 4, after the completion close titanium target power supply.
In embodiments of the present invention, the performance of obtained composite film can be different under different reaction conditions,
When it is implemented, different reaction conditions can be arranged according to different working environments, to obtain the composite membrane of different performance
Layer, to adapt to different working environment demands.
It is specifically described below by following embodiment.
Embodiment 1
Being filled with argon gas to air pressure to vacuum chamber is 0.5Pa, is powered to aluminium target, and adjusting aluminium target power output is 80W, by pre- place
Deposition of aluminum film layer 2 in magnet body 1 after science and engineering skill and coating pre-treatment；Then, being filled with argon gas to air pressure to vacuum chamber is
0.7Pa, radio-frequency power 250W, by radio-frequency sputtering on the aluminum membranous layer 2 of magnet body 1 deposited oxide aluminum membranous layer 3；Finally,
By the indoor gas discharge of vacuum, argon gas and nitrogen are filled with vacuum chamber according to argon flow 30sccm and nitrogen flow 4sccm
Until gas pressure in vacuum is 0.7Pa, adjusting titanium target power is 100W, the depositing titanium nitride in the aluminum oxide film layer 3 of magnet body 1
Film layer 4 closes titanium target power supply after the completion, and through detecting, the performance of the composite film obtained under this condition is as follows: overall film thickness
It is 1.5 μm；Film hardness is 15Gpa；The corrosion-resistant protective performance of film are as follows: at 38 DEG C of temperature, brine strength 5.0% is used
144h, sample non-corroding are continuously stored under spraying test method；Film and substrate combinating strength are Lc=35N；Film carrying
Ability are as follows: surface Vertical loading 2000N, film is without falling off.
Embodiment 2
Being filled with argon gas to air pressure to vacuum chamber is 0.5Pa, is powered to aluminium target, and adjusting aluminium target power output is 100W, by pre-
Deposition of aluminum film layer 2 in magnet body 1 after treatment process and coating pre-treatment；Then, being filled with argon gas to air pressure to vacuum chamber is
1.0Pa, radio-frequency power 350W, by radio-frequency sputtering on the aluminum membranous layer 2 of magnet body 1 deposited oxide aluminum membranous layer 3；Finally,
Vacuum indoor gas is discharged, it is straight that argon gas and nitrogen be filled with vacuum chamber according to argon flow 30sccm and nitrogen flow 4sccm
It is 1.0Pa to gas pressure in vacuum, adjusting titanium target power is 150W, the deposited titanium nitride film in the aluminum oxide film layer 3 of magnet body 1
Layer 4 closes titanium target power supply after the completion, and through detecting, the performance of the composite film obtained under this condition is as follows: overall film thickness is
2.3μm；Film hardness is 22Gpa；The corrosion-resistant protective performance of film are as follows: at 38 DEG C of temperature, brine strength 5.0%, using even
Continue and stores 200h under spraying test method, sample non-corroding；Film and substrate combinating strength are Lc=25N；Film carries energy
Power are as follows: surface Vertical loading 2500N, film is without falling off.
In an alternative embodiment, referring to Fig. 1, in the preparation method 1 surface of magnet be sequentially depositing aluminum membranous layer 2,
Aluminum oxide film layer 3, titanium nitride film 4, specifically includes the following steps:
The pre-sputtering of 10min is carried out before deposition, to target all every time to remove the pollutant of target material surface attachment；
Sample stage baffle is removed, aluminium film 2, pellumina 3, titanium nitride film 4 are sequentially depositing on the magnet 1.
Since metal targets often adhere to the pollutants such as oxide or impurity, so being needed before sputtering sedimentation
Pre-sputtering is carried out to target, pre-sputtering can play the role of cleaning target material surface, prevent the pollutant of target material surface by splashing
It penetrates and deposits to Sintered NdFeB magnet surface, influence the performance of composite film.In pre-sputtering, it can be arranged in sample stage and keep off
Plate, the accumulation of pollutants of target material surface after the completion of pre-sputtering, removes sample to Sintered NdFeB magnet surface when preventing pre-sputtering
Baffle in sample platform carries out sputtering sedimentation titanium nitride film 4 in Sintered NdFeB magnet aluminum oxide film layer 3.
In an alternative embodiment, referring to Fig. 1, the purity of nitrogen can be greater than 99.9wt% in the preparation method,
The purity of argon gas can be greater than 99.9wt%.Important process gas of the argon gas as processes of physical vapor deposition has higher
Purity can make deposition process more stable, so that the deposition of each film layer is stronger not easy to fall off, ensure that compound
The high temperature resistant and corrosion resistance of film layer, in depositing titanium nitride film layer 4, nitrogen is necessary reaction gas, the nitrogen of higher degree
Gas can guarantee sufficiently reacting for titanium and nitrogen in sputtering process, ensure that the purity of titanium nitride film 4, to ensure that compound
The hardness and corrosion resistant degree of corrosion of film layer.
In an alternative embodiment, the purity of aluminium can be greater than 99wt% in the preparation method, and the aluminium of the purity is protected
The quality of aluminum membranous layer 2 after depositing is demonstrate,proved, so that aluminum membranous layer 2 more helps to improve aluminum oxide film layer 3 and magnet as buffer layer
The binding force of ontology 1.
In an alternative embodiment, referring to Fig. 1, the purity of aluminium oxide can be greater than 99wt% in the preparation method,
The fire-resistant oxidation resistant of neodymium iron boron magnetic body can be improved in aluminum oxide film layer 3, and the aluminium oxide of higher degree can make post-depositional
Impurity in aluminum oxide film layer 3 is less, is conducive to the fire-resistant oxidation resistant for improving composite film.
In an alternative embodiment, referring to Fig. 1, titanium purity can be greater than 99wt%, titanium conduct in the preparation method
The purity of the primary raw material of titanium nitride film 4, titanium is bigger, can more reduce the impurity of titanium nitride film 4, so that titanium nitride film
4 hardness and corrosion resistance is higher, to guarantee the hardness and corrosion resistance of the composite film.
The technical principle of the invention is described above in combination with a specific embodiment, these descriptions are intended merely to explain of the invention
Principle shall not be construed in any way as a limitation of the scope of protection of the invention.Based on explaining herein, those skilled in the art
It can associate with other specific embodiments of the invention without creative labor, these modes fall within this hair
Within bright protection scope.
Claims (10)
1. a kind of Sintered NdFeB magnet with composite film, which is characterized in that including magnet body, and stack gradually and set
It is placed in aluminum membranous layer, aluminum oxide film layer and the titanium nitride film on the magnet body surface.
2. the Sintered NdFeB magnet according to claim 1 with composite film, which is characterized in that
The aluminum membranous layer with a thickness of 0.1~0.7 μm；The aluminum oxide film layer with a thickness of 0.1~0.7 μm；The titanium nitride
Film layer with a thickness of 0.4~1.0 μm；
The overall thickness of the composite film is 1.0~2.4 μm.
3. a kind of preparation method of the Sintered NdFeB magnet with composite film, which comprises the following steps:
Magnet body surface is polished, polished and cleaned；
Aluminum membranous layer, aluminum oxide film layer and titanium nitride film are sequentially depositing on the magnet body surface using physical vaporous deposition
Layer.
4. preparation method according to claim 3, which is characterized in that described to be polished magnet body surface, polished
And cleaning includes:
#400, #600, #1000, #1500, #2000 sand paper is utilized respectively successively to polish the surface of the magnet body；
It is polished using surface of the polishing machine to the magnet body that polishing is completed, until it is in mirror-like；
By polishing complete the magnet body be placed sequentially in dehydrated alcohol and acetone soln carry out ultrasonic cleaning 5~
10min, and clean repeatedly twice；
It is put into the vacuum chamber of physical vapor deposition equipment after the magnet body that cleaning terminates is dried,
Starting vacuum pump is evacuated vacuum chamber, and base vacuum is 1 × 10-3Pa, the flow set of argon gas are 10~20sccm, work
Pressure is set as 0.5~1Pa, passes through Ar+ glow discharge effect sputter clean 10~30min further to matrix.
5. preparation method according to claim 3, which is characterized in that described to utilize physical vaporous deposition in the magnet
Body surface is sequentially depositing aluminum membranous layer, aluminum oxide film layer and titanium nitride film
Being filled with argon gas to air pressure to the very described empty room is 0.4~1.0Pa, opens target power supply, adjusts target power output to 80~120W, leads to
Cross magnetron sputtering deposition of aluminum film layer in the processed magnet body；
To the vacuum chamber be filled with argon gas to air pressure be 0.4~1.0Pa, open radio-frequency power supply, adjust radio-frequency power 250W~
400W, by radio-frequency sputtering on the aluminum membranous layer of the magnet body deposited oxide aluminum membranous layer；
The vacuum indoor gas is discharged, is filled with argon gas and nitrogen according to argon flow 30sccm and nitrogen flow 4sccm
The vacuum chamber is until air pressure is 0.4~1.0Pa, and to titanium target energization, adjusting titanium target power is 100~150W, in the magnet
Depositing titanium nitride film layer in the aluminum oxide film layer of ontology closes titanium target power supply after the completion.
6. preparation method according to claim 5, which is characterized in that described to deposit composite anti-corrosive film layer on the magnet
Include:
The pre-sputtering of 10min is carried out before deposition, to target all every time to remove the pollutant of target material surface attachment；
Sample stage baffle is removed, is sequentially depositing aluminium film, pellumina, titanium nitride film on the magnet.
7. preparation method according to claim 5, which is characterized in that the purity of the nitrogen is greater than 99.9wt%, described
The purity of argon gas is greater than 99.9wt%.
8. preparation method according to claim 5, which is characterized in that the aluminium purity is greater than 99wt%.
9. preparation method according to claim 5, which is characterized in that the aluminium oxide purity is greater than 99wt%.
10. preparation method according to claim 5, which is characterized in that the titanium purity is greater than 99wt%.
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