CN105420669B - A kind of CVD method for permanent magnet anti-corrosion pre-treatment - Google Patents
A kind of CVD method for permanent magnet anti-corrosion pre-treatment Download PDFInfo
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- CN105420669B CN105420669B CN201510850389.3A CN201510850389A CN105420669B CN 105420669 B CN105420669 B CN 105420669B CN 201510850389 A CN201510850389 A CN 201510850389A CN 105420669 B CN105420669 B CN 105420669B
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Abstract
A kind of CVD method for permanent magnet anti-corrosion pre-treatment is related to the field of surface treatment of material.The present invention uses physical gas phase deposition technology, and nano-multilayered structures film is deposited on NdFeB surfaces, NdFeB surfaces can be passivated before the step, electrophoresis method depositing coating can be used after the step.Pre-treatment is carried out to NdFeB alloys using gas phase deposition technology the invention discloses one kind, to replace the method for phosphatization.NdFeB magnetic properties caused by can overcoming phosphating process using the technology damage.This method green non-pollution, technological parameter is easily-controllable, and application prospect is extensive.Magnesium-yttrium-transition metal/nitride the composite coating and the binding ability of Nd-Fe-B permanent magnet prepared using this method is excellent, coordinates with electrophoresis or electroplating technology, can significantly improve the decay resistance of Nd-Fe-B permanent magnet.
Description
Technical field
The present invention relates to the field of surface treatment of material, at the surface of neodymium iron boron (NdFeB) permanent-magnet material
Reason technology, specifically, the present invention relates to the preconditioning technique before a kind of permanent-magnet material application.
Background technology
As magnetic material most strong at present, it is all that neodymium iron boron (NdFeB) has been widely used for machinery, medical treatment, automobile etc.
Field, application prospect are very wide.But NdFeB chemical properties are active, it is easy to that corrosion occurs under natural environmental condition, seriously
Hinder its large-scale application.The magnet material of highly corrosion resistant how is obtained, turns into the focus of Recent study.NdFeB be by
The rich Nd and rich B and base phase Nd of thin layer phase2Fe14B is formed.Difference mutually contact with each other, because the difference of electromotive force formed it is countless micro-
Battery, thus corrode, cause magnet the Nomenclature Composition and Structure of Complexes to change, magnetic property declines.
Surface treatment is to improve the main method of NdFeB antiseptic properties.Pass through chemical composition coating, the coat of metal or organic painting
Contact of the barrier air such as layer (or water) with magnet, the service life of magnet can be extended.At present, domestic common commercial scale neodymium
The protective treatment of iron boron surface mainly has phosphorating treatment, plating and electrophoretic coating.Phosphorating treatment is generally as surface preparation;Thereafter
Plating or electrophoretic coating can be used.Electroplating cost is low, but quality stability is poor, and environmental pollution is serious;Electrophoretic coating layer corrosion resistance
Good, environmental pollution is small, is the developing direction of sintered ndfeb permanent magnet body surface treatment.From antiseptic property, simple plating is
Through higher and higher requirement for anticorrosion can not be met, it is necessary to carry out application to neodymium iron boron, and neodymium iron boron needs phosphatization to carry before application
The adhesive force of high paint film.Typical NdFeB anticorrosion process mainly includes following steps:Sealing of hole-passivation-phosphatization-electrophoresis-baking
It is roasting.
Phosphatization be it is a kind of chemistry with electrochemical reaction formed phosphate chemical conversion film process, the phosphate transfection formed
Change film and be referred to as phosphating coat.NdFeB phosphatization includes ferric solid-acid and Zinc phosphating.The purpose of phosphatization is mainly:To parent metal
Protection is provided, prevents metal to be corroded to a certain extent;For preceding bottoming of painting, adhesive force and the anticorrosion of paint film layer are improved
Ability.Phosphatization is conventional pretreatment technology, and after phosphatization, size can increase by 1~10 micron (μm).
The subject matter of phosphatization is magnetic losses be present.With the increase of phosphoric acid concentration, the growth of phosphating time and phosphatization
The raising of temperature, the resistivity increase of soft-magnetic composite material magnetic core, medium-high frequency magnetic loss constantly reduces, while magnetic conductivity also has one
Determine the reduction of degree.Whether phosphating liquor of iron series or Zinc phosphating solution are used, can all damage the magnetic to NdFeB materials.
Current much researchs are directed to the sufacings such as chemical plating, vapour deposition, sol-gel being applied to NdFeB materials
The corrosion protection of material.Protective coating is also developed from initial single coating to multilayer or composite coating.
Gas phase deposition technology includes being divided into physical vapour deposition (PVD) and chemical vapour deposition technique.Wherein physical vapour deposition (PVD) skill
Art includes evaporation coating, sputter coating, ion film plating.Using physical gas phase deposition technology can easily prepare multiple elements design,
Laminated coating.The current report for having vapor deposition of aluminum (Al) coating.After PVD platings Al is carried out on Nd-Fe-B rare-earth permanent magnet surface,
Although plating Al overcoats with excellent antiseptic property, prolonged salt spray test and accelerated corrosion (PCT) experiment can be subjected to,
But because Al is a kind of very low metal of hardness, soft top layer is easy to be scratched, so as to produce local corrosion, and then made
Whole neodymium iron boron magnetic body is corroded.During the carrying and use of neodymium iron boron magnetic body, due to magnet mutual collision and rub
Wipe, frequently result in phenomena such as top layer is scratched, deformed, destroyed, do not had to Fe-B rare-earth permanent magnet so as to plate Al layers
Protective action.Therefore, producing has stronger hardness, while has the neodymium iron boron coating of excellent antisepsis again, tool
It is of practical significance and economic value.
It is higher that the hardness of nano laminated coating is prepared using CVD method, corrosion resistance and good, is to solve above-mentioned ask
The feasible method of topic.
In summary, proposed for the magnetic losses problem of phosphatization pre-treatment, this patent using CVD method pair
NdFeB magnets carry out pre-treatment, and the pre-treatment has good matching with ability cathode electrophoresis.Phosphorization technology can be substituted, overcome
The magnetic loss of phosphorization technology.
The content of the invention
Phosphatization is substituted to carry out pre-treatment to NdFeB permanent magnets using physical gas-phase deposite method the invention provides a kind of
Technical method.
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of Nd-Fe-B permanent magnetic
The preparation method of body surface surface composite coating.This method green non-pollution, technological parameter is easily-controllable, and application prospect is extensive.Using the party
Magnesium-yttrium-transition metal/nitride composite coating and the binding ability of Nd-Fe-B permanent magnet prepared by method is excellent, with electrophoresis or galvanizer
Skill coordinates, and can significantly improve the decay resistance of Nd-Fe-B permanent magnet.
Described technical method, it is characterised in that:
1st, Nd-Fe-B permanent magnet is subjected to surface preparation
(1.1) Nd-Fe-B permanent magnet is subjected to grinding process;
(1.2) Nd-Fe-B permanent magnet in step (1.1) after grinding process is placed in the ultrasonic wave for being loaded with degreasing fluid
Ultrasonic assistant oil removal treatment is carried out in washer;
(1.3) Nd-Fe-B permanent magnet in step (1.2) after ultrasonic assistant oil removal treatment is placed in and is loaded with derusting
Ultrasonic assistant processing of rust removing is carried out in the ultrasonic cleaner of liquid;
(1.4) Nd-Fe-B permanent magnet in step (1.3) after ultrasonic assistant processing of rust removing is placed in going of boiling from
Sealing pores are carried out in sub- water;The time of the sealing pores is 10min~20min.
2nd, the neodymium iron boron magnetic body after surface preparation is subjected to coating film treatment
(2.1) neodymium iron boron magnetic body after the processing of the 1st step is loaded into ion plating equipment vacuum chamber, is evacuated to vacuum<7.6
×10-3Pa。
(2.2) argon gas (Ar) is passed through to 3~4Pa of vacuum.
(2.3) negative bias voltage source is connected, 800~1000V voltages are added between neodymium iron boron magnetic body and vacuum room housing.It is logical
Cross glow discharge sputtering cleaning NdFeB surfaces are purified, activating pretreatment, remove the oil film and oxide-film of magnet surface, time
10~15min.
(2.4) argon gas (Ar) amount is reduced to vacuum 3~5 × 10-1Pa。
(2.5) arc source or sputtering source current, alternating deposit magnesium-yttrium-transition metal and magnesium-yttrium-transition metal nitride are connected.It is only logical
When entering argon gas (Ar), deposited metal;It is passed through argon gas and nitrogen (N2) when, cvd nitride thing.
(2.6) magnesium-yttrium-transition metal includes titanium (Ti), zirconium (Zr), chromium (Cr), tantalum (Ta), hafnium (Hf).
(2.7) during cvd nitride thing, Ar and N are passed through2Intrinsic standoff ratio is 3:1~5:1.
(2.8) deposited metal zirconium or during zirconium nitride, bias is reduced to 70~200V.
(2.9) deposited metal zirconium or during zirconium nitride, depending on sedimentation time is by required film thickness.
(2.10) arc source or sputtering source are closed, closes bias, waiting temperature is reduced at 100 DEG C, takes out magnet.
3. in order to reach corrosion-resistant requirement, depositing coating can be continued using the method for electrophoresis on the vapor deposition layer.
(3.1) magnet after the processing of the 2nd step is put into the tiselius apparatus of epoxy electrophoretic paint.
(3.2) electrophoresis initial voltage 80V~90V, 120~140V of deposition voltage, 2~3min of time, 25~30 DEG C of temperature.
It is 20~30 microns to obtain electrophoretic coating thickness.
(3.3) magnet after electrophoretic process is rinsed in deionized water.
(3.4) baking-curing.First in 80 DEG C of baking 20min of temperature;Then 180 DEG C are increased the temperature to, baking time
20min。
In summary, the present invention uses physical gas phase deposition technology, and nano-multilayered structures film is deposited on NdFeB surfaces,
NdFeB surfaces can be passivated before the step, electrophoresis method depositing coating can be used after the step.With existing NdFeB anti-corrosion sides
Phosphatization in method is compared, and is had the following advantages that:
(1) magnetic property of NdFeB magnets is not damaged.Overcome parkerized magnetic loss and hinder shortcoming.
(2) it is free from environmental pollution.Gas phase deposition technology overcomes the shortcomings that parkerized contaminated wastewater environment, is a kind of green
Technology that color is pollution-free.
(3) decay resistance of NdFeB magnets is improved.Gas phase deposition technology can easily prepare multicomponent, nanometer
Multilayer, composite coating.Coating is fine and close, can completely cut off extraneous corrosive medium and be contacted with NdFeB;Can prepare nitride ceramics coating with
The good metal coating of corrosion resistance.
(4) hardness of nano laminated coating is higher, improves the ability of the anti-foreign object damage of magnet.
(5) it is strong with the adhesion of the post-treatment coatings such as electrophoresis.
Brief description of the drawings
Fig. 1 is the structure of NdFeB magnets, vapour deposition Zr/ZrN multilayer films and electrophoretic painting layer in specific embodiment one
Schematic diagram.
Fig. 2 is Zr/ZrN films Cross Section Morphology in specific embodiment one.It can be seen that about 1 micron of the thickness of film.
Fig. 3 is current potential-current curve of Zr/ZrN films in specific embodiment one.Show the decay resistance of film compared with
It is good.
Fig. 4 is the Cross Section Morphology of Ti/TiN films in specific embodiment two.Example three is similar with the Cross Section Morphology of the film of example two.
Surface roughness is favorably improved follow-up application bond strength.
Fig. 5 is the electrode-electric position curve of Ti/TiN films in specific embodiment two.Show the decay resistance of film compared with
It is good.
Fig. 6 is electrode-electric position curve of the specific embodiment three using electrochemical workstation test Cr/CrN films.
Embodiment
Technical scheme, but protection scope of the present invention not limited to this are illustrated with specific embodiment below:
Embodiment one:
In this embodiment, using magnetron sputtering technique, using NdFeB magnets as matrix, sputtering sedimentation zirconium (Zr) and nitridation
The film of the nano-multilayered structures of zirconium (ZrN).Specific preparation process is as follows:
(1) pre-treatment:Nd-Fe-B permanent magnet is subjected to grinding process;Nd-Fe-B permanent magnet after grinding process is placed in Sheng
Ultrasonic assistant oil removal treatment is carried out in ultrasonic cleaner equipped with degreasing fluid;By the neodymium after ultrasonic assistant oil removal treatment
Iron boron permanent magnet is placed in progress ultrasonic assistant processing of rust removing in the ultrasonic cleaner for be loaded with rust removing solution;Through ultrasonic assistant
Nd-Fe-B permanent magnet after processing of rust removing, which is placed in the deionized water boiled, carries out sealing pores;The time of the sealing pores is
10 minutes.
(2) magnetron sputtering apparatus vacuum chamber is put into after drying.Film is vacuumized to vacuum 7 × 10-3Pa.It is passed through argon gas (Ar)
To vacuum 3Pa.Negative bias voltage source is connected, 800 volts of voltages are added between neodymium iron boron magnetic body and vacuum room housing.Pass through brightness
Light sputter clean is purified to NdFeB surfaces, activating pretreatment, removes the oil film and oxide-film of magnet surface, and the time 10 divides
Clock.
(3) argon gas (Ar) amount is reduced to vacuum 3 × 10-1Pa。
(4) sputtering source current, deposition magnesium-yttrium-transition metal zirconium (Zr) are opened.Bias is reduced to 70V, 15 minutes time.
(5) keep zirconium sputtering source to open, be passed through nitrogen (N2) to vacuum 4 × 10-1Pa, now Ar and N2Intrinsic standoff ratio is 3:
1.Cvd nitride zirconium (ZrN) layer is to thickness about 70nm.
(6) keep zirconium sputtering source to open, close nitrogen, deposited metal zirconium (Zr) layer to thickness about 45nm.
(7) repetition the 5th, 6 steps, totally 8 times.
(8) sputtering source is closed, closes nitrogen, argon gas.
(9) vacuum room temperature is waited to be reduced to 100 degree.Magnet is taken out in blow-on.
(10) magnet is put into the tiselius apparatus of epoxy electrophoretic paint.Electrophoresis initial voltage 80V, deposition voltage 120V, time
2min, 25 DEG C of temperature.It is 20 microns to obtain electrophoretic coating thickness.
(11) magnet after electrophoretic process is rinsed in deionized water.
(12) baking-curing.First in 80 DEG C of baking 20min of temperature;Then 180 DEG C are increased the temperature to, baking time 20min.
Fig. 1 is the structural representation of NdFeB magnets, vapour deposition Zr/ZrN multilayer films and electrophoretic painting layer.
Fig. 2 is to use scanning electron microscopic observation Zr/ZrN film Cross Section Morphologies.It can be seen that about 1 micron of the thickness of film.
Fig. 3 is current potential-current curve using electrochemical workstation test Zr/ZrN films.It can be seen that the current potential of film compared with
It is negative, and in 30min inner potentials without significant changes;Show that the decay resistance of film is preferable.
Embodiment two:
In this embodiment, using arc ion plating (aip), using NdFeB magnets as matrix, titanium deposition (Ti) and titanium nitride
(TiN) film of nano-multilayered structures.Specific preparation process is as follows:
(1) pre-treatment:Nd-Fe-B permanent magnet is subjected to grinding process;Nd-Fe-B permanent magnet after grinding process is placed in Sheng
Ultrasonic assistant oil removal treatment is carried out in ultrasonic cleaner equipped with degreasing fluid;By the neodymium after ultrasonic assistant oil removal treatment
Iron boron permanent magnet is placed in progress ultrasonic assistant processing of rust removing in the ultrasonic cleaner for be loaded with rust removing solution;Through ultrasonic assistant
Nd-Fe-B permanent magnet after processing of rust removing, which is placed in the deionized water boiled, carries out sealing pores;The time of the sealing pores is
20 minutes.
(2) arc ion plating apparatus vacuum chamber is put into after drying.Film is vacuumized to vacuum 7 × 10-3Pa.It is passed through argon gas
(Ar) is to vacuum 4Pa.Negative bias voltage source is connected, 1000 volts of voltages are added between neodymium iron boron magnetic body and vacuum room housing.
NdFeB surfaces are purified by glow discharge sputtering cleaning, activating pretreatment, remove the oil film and oxide-film of magnet surface, when
Between 15 minutes.
(3) argon gas (Ar) amount is reduced to vacuum 5 × 10-1Pa。
(4) arc power, deposition magnesium-yttrium-transition metal titanium (Ti) are opened.Bias is reduced to 200V.2 minutes time.
(5) keep titanium arc source to open, be passed through nitrogen (N2) to vacuum 6 × 10-1Pa, now Ar and N2Intrinsic standoff ratio is 5:
1.Depositing titanium nitride (TiN) layer is to thickness about 40nm.
(6) keep titanium arc source to open, close nitrogen, deposited metal titanium (Ti) layer to thickness about 30nm.
(7) repetition the 5th, 6 steps, totally 20 times.
(8) arc source is closed, closes nitrogen, argon gas.
(9) vacuum room temperature is waited to be reduced to 100 degree.Magnet is taken out in blow-on.
(10) magnet is put into the tiselius apparatus of epoxy electrophoretic paint.Electrophoresis initial voltage 85V, deposition voltage 130V, time
2.5min, 28 DEG C of temperature.It is 25 microns to obtain electrophoretic coating thickness.
(11) magnet after electrophoretic process is rinsed in deionized water.
(12) baking-curing.First in 80 DEG C of baking 20min of temperature;Then 180 DEG C are increased the temperature to, baking time 20min.
Fig. 4 is the Cross Section Morphology of coating after arc deposited Ti/TiN.The surface roughness of arc deposited coating is splashed compared with magnetic control
Penetrate the adhesion for greatly, being favorably improved follow-up electrophoretic painting.
Fig. 5 is the electrode-electric position curve using electrochemical workstation test Ti/TiN films.It can be seen that the current potential of film compared with
It is negative, and in 30 minutes, membrane potential varies slightly, and shows that film has preferable decay resistance.
Embodiment three
In this embodiment, using magnetron sputtering technique, using NdFeB magnets as matrix, sputtering sedimentation chromium (Cr) and nitridation
The film of the nano-multilayered structures of chromium (CrN).Specific preparation process is as follows:
(1) pre-treatment:Nd-Fe-B permanent magnet is subjected to grinding process;Nd-Fe-B permanent magnet after grinding process is placed in Sheng
Ultrasonic assistant oil removal treatment is carried out in ultrasonic cleaner equipped with degreasing fluid;By the neodymium after ultrasonic assistant oil removal treatment
Iron boron permanent magnet is placed in progress ultrasonic assistant processing of rust removing in the ultrasonic cleaner for be loaded with rust removing solution;Through ultrasonic assistant
Nd-Fe-B permanent magnet after processing of rust removing, which is placed in the deionized water boiled, carries out sealing pores;The time of the sealing pores is
20 minutes.
(2) magnetron sputtering apparatus vacuum chamber is put into after drying.Film is vacuumized to vacuum 7 × 10-3Pa.It is passed through argon gas (Ar)
To vacuum 3.5Pa.Negative bias voltage source is connected, 900 volts of voltages are added between neodymium iron boron magnetic body and vacuum room housing.Pass through
Glow discharge sputtering cleaning is purified to NdFeB surfaces, activating pretreatment, removes the oil film and oxide-film of magnet surface, time 12
Minute.
(3) argon gas (Ar) amount is reduced to vacuum 4 × 10-1Pa。
(4) magnetron sputtering power supply, deposition magnesium-yttrium-transition metal titanium (Ti) are opened.Bias is reduced to 150V.3 minutes time.
(5) keep titanium sputtering source to open, be passed through nitrogen (N2) to vacuum 5 × 10-1Pa, now Ar and N2Intrinsic standoff ratio is 4:
1.Depositing titanium nitride (ZrN) layer is to about 60 nanometers of thickness..
(6) keep titanium sputtering source to open, close nitrogen, deposited metal titanium (Ti) layer to about 50 nanometers of thickness.
(7) repetition the 5th, 6 steps, totally 20 times.
(8) sputtering source is closed, closes nitrogen, argon gas.
(9) vacuum room temperature is waited to be reduced to 100 degree.Magnet is taken out in blow-on.
(10) magnet is put into the tiselius apparatus of epoxy electrophoretic paint.Electrophoresis initial voltage 90V, deposition voltage 140, time
3min, 30 DEG C of temperature.It is 30 microns to obtain electrophoretic coating thickness.
(11) magnet after electrophoretic process is rinsed in deionized water.
(12) baking-curing.First in 80 DEG C of baking 20min of temperature;Then 180 DEG C are increased the temperature to, baking time 20min.
Fig. 6 is the electrode-electric position curve using electrochemical workstation test Cr/CrN films.It can be seen that the current potential of film compared with
It is negative, and in 30 minutes, membrane potential varies slightly, and shows that film has preferable decay resistance.
Claims (1)
1. a kind of CVD method for permanent magnet anti-corrosion pre-treatment, it is characterised in that comprise the following steps:
1) Nd-Fe-B permanent magnet, is subjected to surface preparation
(1.1) Nd-Fe-B permanent magnet is subjected to grinding process;
(1.2) Nd-Fe-B permanent magnet in step (1.1) after grinding process is placed in the ultrasonic wave cleaning for being loaded with degreasing fluid
Ultrasonic assistant oil removal treatment is carried out in device;
(1.3) Nd-Fe-B permanent magnet in step (1.2) after ultrasonic assistant oil removal treatment is placed in and is loaded with rust removing solution
Ultrasonic assistant processing of rust removing is carried out in ultrasonic cleaner;
(1.4) Nd-Fe-B permanent magnet in step (1.3) after ultrasonic assistant processing of rust removing is placed in the deionized water boiled
Middle carry out sealing pores;The time of the sealing pores is 10min~20min;
2) neodymium iron boron magnetic body after surface preparation, is subjected to coating film treatment
(2.1) by the 1st) step processing after neodymium iron boron magnetic body load ion plating equipment vacuum chamber, be evacuated to vacuum<7.6×
10-3Pa;
(2.2) argon gas is passed through to 3~4Pa of vacuum;
(2.3) negative bias voltage source is connected, 800~1000V voltages are added between neodymium iron boron magnetic body and vacuum room housing;Pass through brightness
Light sputter clean is purified to NdFeB surfaces, activating pretreatment, removes the oil film and oxide-film of magnet surface, and the time 10~
15min;
(2.4) argon gas amount is reduced to vacuum 3~5 × 10-1Pa;
(2.5) arc source or sputtering source current, alternating deposit magnesium-yttrium-transition metal and magnesium-yttrium-transition metal nitride are connected;Only it is passed through argon
During gas, deposited metal;When being passed through argon gas and nitrogen, cvd nitride thing;The magnesium-yttrium-transition metal includes titanium, zirconium, chromium, tantalum and hafnium;
During cvd nitride thing, Ar and N are passed through2Intrinsic standoff ratio is 3:1~5:1;When deposited metal zirconium or zirconium nitride, bias is reduced to 70~
200V;
Deposition closes arc source or sputtering source after terminating, and closes bias, and waiting temperature is reduced at 100 DEG C, takes out magnet;
3) depositing coating, is continued using the method for electrophoresis on the vapor deposition layer
(3.1) by the 2nd) step processing after magnet be put into the tiselius apparatus of epoxy electrophoretic paint;
(3.2) electrophoresis initial voltage 80V~90V, 120~140V of deposition voltage, 2~3min of time, 25~30 DEG C of temperature;Obtain
Electrophoretic coating thickness is 20~30 microns;
(3.3) magnet after electrophoretic process is rinsed in deionized water;
(3.4) baking-curing;First in 80 DEG C of baking 20min of temperature;Then 180 DEG C are increased the temperature to, baking time 20min.
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