CN105803408A - Neodymium-iron-boron permanent magnet surface protection method - Google Patents
Neodymium-iron-boron permanent magnet surface protection method Download PDFInfo
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- CN105803408A CN105803408A CN201410833542.7A CN201410833542A CN105803408A CN 105803408 A CN105803408 A CN 105803408A CN 201410833542 A CN201410833542 A CN 201410833542A CN 105803408 A CN105803408 A CN 105803408A
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Abstract
The invention provides a neodymium-iron-boron permanent magnet surface protection method. The method comprises 1, material polishing: carrying out conventional polishing on a permanent magnetism material, 2, degreasing oil removal: adding an alkaline solution into the polished permanent magnetism material and carrying out conventional degreasing oil removal, 3, conventional rust removal utilizing wet method sandblasting, 4, vacuum magnetron sputtering aluminum deposition and 5, vacuum plating of an aluminum trioxide protection layer. Through vacuum magnetron sputtering aluminum and aluminum trioxide plating, a neodymium-iron-boron permanent magnet vacuum aluminum plating binding force is improved and corrosion resistance is improved.
Description
Technical field
The present invention relates to the anti-corrosion method of Nd-Fe-B permanent magnet material, specifically, relate to the method for protecting surface of a kind of Nd-Fe-B permanent magnet.
Background technology
The application of neodymium iron boron (NdFeB) permanent magnet material in recent years and development are very rapid, and the protection success or not of Nd-Fe-B permanent magnet material be related to material can one of the key technology of popularization and application.This material is mainly prepared from by powder metallurgical technique by elements such as rare earth metal neodymium Nd, ferrum and boron.As magnetic material the strongest at present, having been widely used for all fields such as electroplating device, machinery, medical treatment, automobile, application prospect is very wide.
The premise of Nd-Fe-B permanent magnet material application is to first have to resolve the Anticorrosion of Nd-Fe-B permanent magnet material.As the porous material that a kind of powder metallurgical technique is prepared from, because of rich neodymium phase therein, neodymium iron boron principal phase and border are readily formed intercrystalline corrosion mutually.Rear earth element nd in neodymium iron boron powder metallurgy, character is active, the corrosion resisting property making whole Nd Fe B alloys becomes very poor, very easily corrosion in damp and hot environment, because corrosion failure causes decline or the damage of magnetic property, have a strong impact on the service life of Nd-Fe-B permanent magnet, reduce stability and the reliability of product.The magnetic property of Nd-Fe-B permanent magnet material and its organizational structure have very big relation.The principal phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property.Coercivity contribution is maximum is rich neodymium phase.To there is huge change in the magnetic property of material after corrosion occurs Nd-Fe-B permanent magnet material.Therefore, the Anticorrosion of Nd-Fe-B permanent magnet material is always up the subject matter that Nd-Fe-B permanent magnet material needs to solve.
The anti-corrosion method of current Nd-Fe-B permanent magnet material has a lot.Wherein there are electronickelling, electrogalvanizing (CN1421547A, CN1056133A), shooting of multi-layer nickel electroplating (CN102568732), copper facing (CN1514889A), the multiple method such as phosphatization (CN101022051), vacuum aluminum-coated (CN101736304A, CN101724820B).CN101736304A vacuum aluminizing method of surface of neodymium-iron-boron permanent magnet, wherein, in turn includes the following steps: (1) adopts wet-tumbling cleaning surface of Nd-Fe-B permanent magnet；(2) Nd-Fe-B permanent magnet is put on the rotational workpieces frame in coating chamber, make Nd-Fe-B permanent magnetic temperature be maintained between 250-300 DEG C；(3) start the vacuum pump on coating chamber, the vacuum in coating chamber is adjusted to 1-9 × 10-3 handkerchief；(4) start the magnetic control multi arc sputtering that the multi sphere cathode evaporator of coating chamber both sides, planar magnetic sputtering target and rotational workpieces frame carry out 2-7 hour simultaneously；(5) after maintenance coating chamber cools down 30-60 minute under vacuo, inflate blow-on, take out the Nd-Fe-B permanent magnet aluminized, carry out chromium-free passivation liquid passivation.The high energy ion that magnetron sputtering produces, clashes into the low energy ion that multi sphere method produces, promotes the more ionizing of the latter, and both speed tend to unified, and efficiency improves.Neodymium iron boron is carried out anticorrosion by the mode adopting multi-arc ion coating.The mode of its multi-arc ion coating adopted very easily produces big granule, and antiseptic property is poor, and the time is also long.CN101724820B relates to a kind of method of magnetron sputtering deposition of aluminum film for surface protection of NdFeB workpiece, it is characterized in that: comprise the steps: that (1) is at the vacuum indoor location purity aluminum target more than 98% so that it is and the angle of horizontal plane is between 45 °～90 °；(2) neodymium iron boron workpiece is carried out oil removing, processing of rust removing；(3) neodymium iron boron workpiece is placed on work supporting block；(4) evacuation, makes the vacuum in vacuum chamber be not more than 1 × 10-3Pa；(5) neodymium iron boron workpiece is carried out sputtering sedimentation aluminum film, employing noble gas is working gas, and operating air pressure is 0.1～10Pa, and the sputtering power of unit target area is 1～6w/cm2, adopting at least one aluminum target that neodymium iron boron workpiece is sputtered, sputtering time is 1～5h；(6) Manual manipulator upset neodymium iron boron workpiece is adopted；(7) neodymium iron boron workpiece is carried out sputtering sedimentation, employing noble gas is working gas, and operating air pressure is 0.1～10Pa, and the sputtering power of unit target area is 1～6w/cm2, adopting at least one sputtering target that neodymium iron boron workpiece is sputtered, sputtering time is 1～5 hour.
Aluminum is that a kind of amphoteric metal all very easily corrodes under acid condition and alkali condition, the passivation therefore product being correlated with after plating.It is generally adopted chemical method and aluminum is carried out trivalent chromium passivation.And the present invention adopts the method for vapour deposition to carry out vacuum moulding machine aluminum oxide coating on aluminium lamination surface can effectively improve the anticorrosion ability of aluminium coat.It addition, magnetron sputtering is under the action of a magnetic field now, spin up, bombardment, on target, makes the effective rate of utilization of target lower than 20%, in order to improve target effective rate of utilization, Target Design is become convex by the present invention, consistent with magnetic field acceleration orbit, improves the utilization rate of target.In vacuum aluminum-coated, adopt unidirectional current can obtain aluminium lamination of good performance, but when being mixed into oxygen in target chamber, target can poison, the effect that impact is aluminized.Therefore, in plating aluminium sesquioxide process, central want Switching power, changed into radio frequency, it is possible to obtain the coating of function admirable.
Summary of the invention
In order to solve problem of the prior art, it is an object of the invention to provide the method for protecting surface of a kind of Nd-Fe-B permanent magnet, to overcome defect of the prior art.
Method for protecting surface of the present invention comprises the steps: that (1) material polishes: described permanent magnet material carries out conventional polishing；(2) degreasing degreasing: add alkaline solution and grinded permanent magnet material is carried out conventional degreasing degreasing；(3) vapour blasting is adopted to carry out conventional rust cleaning；(4) adopt vacuum magnetic-control sputtering deposition of aluminum: under vacuum inert gas shielding, adopt DC source, the vacuum sintering furnace of temperature 230-250 DEG C carries out magnetron sputtering and aluminizes, obtain aluminium lamination；And (5) Vacuum Deposition three aoxidizes three aluminum protective layers: passing into oxygen, oxygen and inert gas ratio is 1:3～5, adopts radio-frequency power supply under vacuo, at temperature 200～230 DEG C, carry out magnetron sputtering aluminium sesquioxide layer, aluminum layer thickness 1 micron.Wherein, described noble gas is argon.
In the preferred technical solution of the present invention, step (4) vacuum is 1.0*10-4Pa.It is highly preferred that the DC source in step (4) is 400～450 volts of back bias voltages.The time of aluminizing in step (4) is 160～300 points.The aluminum layer thickness obtained in step (4) is 3-10 micron.
In the preferred technical solution of the present invention, the vacuum in step (5) is 0.06～10 handkerchief.It is highly preferred that the 600 volts of back bias voltages of radio-frequency power supply in step (5).The aluminium sesquioxide layer thickness that step (5) obtains is 1～3 micron.
In the preferred technical solution of the present invention, adopting magnetic controlled sputtering target to carry out magnetron sputtering and aluminize, described magnetic controlled sputtering target is arc-shaped.
In the preferred technical solution of the present invention, described permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
The present invention adopts the mode of magnetron sputtering vacuum plating aluminum and aluminium sesquioxide not only to improve the vacuum aluminum-coated adhesion of Nd-Fe-B permanent magnet but also improves antiseptic property.
Accompanying drawing explanation
Fig. 1 represents the shape graph of target of the present invention；
Fig. 2 represents prior art target；
Fig. 3 represents the target working state schematic representation of the present invention.
Detailed description of the invention
For making auditor can further appreciate that the structure of the present invention, feature and other purposes, it is accompanied by accompanying drawing in conjunction with appended preferred embodiment and describes in detail as follows, use this accompanying drawing embodiment described to be merely to illustrate technical scheme the non-limiting present invention.
Embodiment 1
First by 2.5kg'sSintered Nd-Fe-B permanent magnetic material machinery vibration 2 hours in vibrating ball-mill, then with alkaline solution (sodium phosphate 20g/L, sodium carbonate 10g/L and sodium hydroxide 10g/L) degreasing degreasing, subsequently acid pickling and rust removing in the salpeter solution of 1%.Carry out wet blast-cleaning again.
The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, it is filled with argon to 25 handkerchiefs, adopts 400 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminize the time 160 points, aluminum layer thickness 1.2 microns.Passing into oxygen, oxygen and argon ratio is 1:5, house vacuum degree 5 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 230 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 1 micron.Refer to table 1.
Embodiment 2
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-3Pa.With argon for working gas, it is filled with argon to 15 handkerchiefs, adopts 450 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminize the time 200 points, aluminum layer thickness 3 microns.Passing into oxygen, oxygen and argon ratio is 1:4, house vacuum degree 5 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 230 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 2 microns.Refer to table 1.
Embodiment 3
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, it is filled with argon to 25 handkerchiefs, adopts 400 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminize the time 300 points, aluminum layer thickness 1.0 microns.Passing into oxygen, oxygen and argon ratio is 1:4.5, house vacuum degree 5 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 230 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 3 microns.Refer to table 1.
Embodiment 4
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, it is filled with argon to 25 handkerchiefs, adopts 400 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminize the time 200 points, aluminum layer thickness 1.2 microns.Passing into oxygen, oxygen and argon ratio is 1:3.5, house vacuum degree 5 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 230 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 2 microns.Refer to table 1.
Embodiment 5
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, it is filled with argon to 25 handkerchiefs, adopts 400 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminize the time 200 points, aluminum layer thickness 1.0 microns.Passing into oxygen, oxygen and argon ratio is 1:3, house vacuum degree 0.06 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 230 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 2 microns.Refer to table 1.
Embodiment 6
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, it is filled with argon to 25 handkerchiefs, adopts 400 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminize the time 250 points.It is 1:5 that aluminum layer thickness 2.5 microns passes into oxygen, oxygen and argon ratio, house vacuum degree 0.5 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 200 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 2.5 microns.Refer to table 1.
Embodiment 7
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, it is filled with argon to 25 handkerchiefs, adopts 400 volts of back bias voltages of DC source, temperature 250 degree, Magnetron Sputtered Al in vacuum sintering furnace.Aluminum layer thickness 1.5 microns is aluminized the time 240 points.Passing into oxygen, oxygen and argon ratio is 1:4, house vacuum degree 10 handkerchief, adopts 600 volts of back bias voltages of radio-frequency power supply, temperature 230 degree, magnetron sputtering aluminium sesquioxide, aluminum layer thickness 2.1 microns.Refer to table 1.
Comparative example 1
According to the method for embodiment 1 to 2.5kg'sNd-Fe-B permanent magnet material carry out surface pretreatment.Carry out wet blast-cleaning again.The neodymium iron boron workpiece of drying is suspended in vacuum chamber, is evacuated down to 10Pa with mechanical pump, then use turbomolecular pump evacuation, make the vacuum of vacuum chamber reach 1.0*10-4Pa.With argon for working gas, adopting ion source that neodymium iron boron workpiece surface is carried out, regulate anode voltage 120 volts, electric current 1.0 is pacified, and carries out vacuum sputtering and aluminizes, and aluminizes the time 300 points.Refer to table 1.
Table 1
| Embodiment number | Plating thick (micron) | Salt fog (hour) |
| Embodiment 1 | 10.0 | 120 |
| Embodiment 2 | 9.7 | 120 |
| Embodiment 3 | 10.2 | 120 |
| Embodiment 4 | 9.8 | 120 |
| Embodiment 5 | 10.0 | 120 |
| Embodiment 6 | 10.4 | 120 |
| Embodiment 7 | 10.2 | 120 |
| Comparative example 1 | 12.1 | 96 |
Fig. 2 is the aluminum target shape of prior art, the target shape graph of Fig. 1 and Fig. 3 respectively technical solution of the present invention and working state schematic representation.Contrasted it can be seen that stock utilization is enhanced about more than once by Fig. 1 and Fig. 2 target.As seen from Figure 1, the middle electronics of magnetron sputtering accelerates arc orbit design, and aluminium can be fully utilized.Normal aluminum target is except arc orbit, and remainder is all without being fully used.And adopt the target such as Fig. 1 mode stock utilization to be enhanced about more than once.
It should be noted that foregoing invention content and detailed description of the invention are intended to prove the practical application of technical scheme provided by the present invention to should not be construed as limiting the scope of the present invention.Those skilled in the art are in the spirit and principle of the present invention, when doing various amendment, equivalent replacement or improve.Protection scope of the present invention is as the criterion with appended claims.
Claims (10)
1. the surface treatment method of a permanent magnet material, it is characterised in that described surface treatment method comprises the steps:
(1) material polishing: described permanent magnet material is carried out conventional polishing；
(2) degreasing degreasing: add alkaline solution and grinded permanent magnet material is carried out conventional degreasing degreasing；
(3) vapour blasting is adopted to carry out conventional rust cleaning；
(4) adopt vacuum magnetic-control sputtering deposition of aluminum: under vacuum inert gas shielding, adopt DC source, the vacuum sintering furnace of temperature 230-250 DEG C carries out magnetron sputtering and aluminizes, obtain aluminium lamination；And
(5) Vacuum Deposition three aoxidizes three aluminum protective layers: passing into oxygen, oxygen and inert gas ratio is 1:3～1:5, adopts radio-frequency power supply under vacuo, carries out magnetron sputtering aluminium sesquioxide layer, aluminum layer thickness 1-3 micron at temperature 200～230 DEG C.
2. surface treatment method according to claim 1, it is characterised in that step (4) vacuum is 1.0*10-4-1.0*10-3Pa。
3. surface treatment method according to claim 1, it is characterised in that the DC source in step (4) is 400～450 volts of back bias voltages.
4. surface treatment method according to claim 1, it is characterised in that the time of aluminizing in step (4) is 160～300 points.
5. surface treatment method according to claim 1, it is characterised in that the vacuum in step (5) is 0.06～10 handkerchief.
6. surface treatment method according to claim 1, it is characterised in that 600 volts of back bias voltages of the radio-frequency power supply in step (5).
7. surface treatment method according to claim 1, it is characterised in that the aluminum layer thickness obtained in step (4) is 3-10 micron；The aluminium sesquioxide layer thickness that step (5) obtains is 1～3 micron.
8. surface treatment method according to claim 1, it is characterised in that described noble gas is argon.
9. surface treatment method according to claim 1, it is characterised in that adopting magnetic controlled sputtering target to carry out magnetron sputtering and aluminize, described magnetic controlled sputtering target is arc-shaped.
10. according to the arbitrary described surface treatment method of claim 1～9, it is characterised in that described permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108447670A (en) * | 2018-01-12 | 2018-08-24 | 浙江鑫盛永磁科技有限公司 | A kind of preparation method of used in high-speed motor permanent magnet ndfeb composite magnetic steel |
| CN109346306A (en) * | 2018-10-26 | 2019-02-15 | 合肥工业大学 | A kind of In-situ reaction coating and preparation method thereof for neodymium iron boron magnetic body surfacecti proteon |
| CN110699648A (en) * | 2019-10-11 | 2020-01-17 | 宁波韵升股份有限公司 | PVD composite film layer of neodymium iron boron magnet and preparation process |
| CN113564548A (en) * | 2021-06-22 | 2021-10-29 | 杭州电子科技大学 | Method for improving corrosion resistance of sintered neodymium iron boron |
| CN115011937A (en) * | 2021-03-06 | 2022-09-06 | 东莞市峰谷纳米科技有限公司 | Surface oxidation method |
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| CN102400091A (en) * | 2010-09-10 | 2012-04-04 | 鸿富锦精密工业（深圳）有限公司 | Surface treatment method for aluminum alloy and housing prepared from aluminum alloy |
| CN102485938A (en) * | 2010-12-01 | 2012-06-06 | 鸿富锦精密工业（深圳）有限公司 | Part coated with anti-fingerprint coating and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108447670A (en) * | 2018-01-12 | 2018-08-24 | 浙江鑫盛永磁科技有限公司 | A kind of preparation method of used in high-speed motor permanent magnet ndfeb composite magnetic steel |
| CN109346306A (en) * | 2018-10-26 | 2019-02-15 | 合肥工业大学 | A kind of In-situ reaction coating and preparation method thereof for neodymium iron boron magnetic body surfacecti proteon |
| CN110699648A (en) * | 2019-10-11 | 2020-01-17 | 宁波韵升股份有限公司 | PVD composite film layer of neodymium iron boron magnet and preparation process |
| CN115011937A (en) * | 2021-03-06 | 2022-09-06 | 东莞市峰谷纳米科技有限公司 | Surface oxidation method |
| CN113564548A (en) * | 2021-06-22 | 2021-10-29 | 杭州电子科技大学 | Method for improving corrosion resistance of sintered neodymium iron boron |
| CN113564548B (en) * | 2021-06-22 | 2023-12-08 | 杭州电子科技大学 | Method for improving corrosion resistance of sintered NdFeB |
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