CN102191464B - Anticorrosion coating for neodymium-iron-boron rare earth permanent magnet and manufacturing method thereof - Google Patents
Anticorrosion coating for neodymium-iron-boron rare earth permanent magnet and manufacturing method thereof Download PDFInfo
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- CN102191464B CN102191464B CN201010119342.7A CN201010119342A CN102191464B CN 102191464 B CN102191464 B CN 102191464B CN 201010119342 A CN201010119342 A CN 201010119342A CN 102191464 B CN102191464 B CN 102191464B
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Abstract
The invention relates to a coating for a neodymium-iron-boron aluminum-based alloy and a manufacturing method thereof, wherein the coating has excellent anticorrosion properties and higher hardness. The coating for the aluminum-based alloy comprises an inner layer and an outermost layer, wherein the inner layer consists of an aluminum-based alloy coating A or B which comprises the component of Al100-x-Mx; and the outermost layer consists of an oxide layer alloy which comprises the component of (Al100-x-Mx)2O3, wherein M is one or more of Cr, Co, Mo, W, Zr, Ti, Nb and Mn elements, and x is more than or equal to 0.05 and is less than or equal to 10, and is average atomic percent. The coating is obtained through treatment by a vapor deposition process or a sputtering process, has the characteristics of higher hardness, strong bonding force, high compactness and the like, and can better protect neodymium-iron-boron magnets from being corroded to the maximum extent.
Description
Technical field
The present invention relates to the surface anticorrosion coating of permanent-magnet rare-earth NdFeB alloy, and the method for manufacturing this coating for protection against corrosion is provided.
Background technology
Fe-B rare-earth permanent magnet is to have excellent magnetic property, is widely used in the fields such as electronics, motor, communication! But the feature of its corrosion-resistant makes, it is easy to get rusty, efflorescence, thereby loses efficacy.Generally need to can use at surface coverage one deck coating for protection against corrosion of NdFeB rear-earth magnet.Common coating comprises phosphate coating, electro-galvanized layer, electroplated Ni layer and physical vapor deposition (PVD) plating Al layer etc. at present! Wherein PVD plating Al is because its antiseptic property is excellent, flux loss is little and environmental protection comes into one's own, and refers to You Heqi army and Li Wei in Metallic Functional Materials, vol8, No.5, " the Nd-Fe-Bo permanent magnet material protection against corrosion researchdevelopment " delivered on 2001.
On Nd-Fe-B rare-earth permanent magnet surface, carry out after PVD plating Al, although plating Al protective layer has excellent antiseptic property, can stand long salt-fog test and accelerated corrosion (PCT) test, but because Al is the metal that a kind of hardness is very low, soft top layer is easy to be scratched, thereby generation local corrosion, and then whole neodymium iron boron magnetic body is corroded! In the carrying and use procedure of neodymium iron boron magnetic body, due to mutual collision and the friction of magnet, often cause the phenomenons such as top layer is scratched, distortion, thereby plating Al layer is damaged, and does not have the protective effect to Fe-B rare-earth permanent magnet.Therefore, produce and there is stronger hardness, can stand the collision in handling process, opposing, the while has again the neodymium iron boron coating of excellent preservative activity, has practical significance and economic worth.
Summary of the invention
In view of the above problems, the object of the present invention is to provide and a kind ofly there is excellent protective effect and compared with the coating of the Fe-B rare-earth permanent magnet of strong hardness and manufacture method thereof, in order to prevent that neodymium iron boron magnetic body is corroded.
The present invention, by physical vapor deposition, adopts the method for evaporation or sputter aluminum base alloy, at the plated surface last layer aluminum base alloy coating of Fe-B rare-earth permanent magnet.According to an aspect of the present invention, the invention provides a kind of aluminum base alloy coating with good Anticorrosive Character and harder neodymium iron boron, the component of described aluminum base alloy coating is Al
100-x-M
x; Wherein, M comprises Cr, Co, Mo, W, Zr, Ti, Nb, one or more elements in Mn element; 0.05≤x≤10, x is average atom per-cent.
Preferably, M is Cr and be selected from Co, Mo, W, Zr, Ti, Nb, a kind of in Mn element.
Preferably, the thickness of described aluminum base alloy coating is respectively 5～30 μ m.
Preferably, described aluminum base alloy coating also comprises an adventitia, and described adventitia is (Al by component
100-x-M
x)
2o
3form, wherein, M comprises Cr, Co, Mo, W, Zr, Ti, Nb, one or more elements in Mn element; 0.05≤x≤10, x is average atom per-cent.Oxygen be mainly in coating passivating process, introduce or coating form after because oxygenizement is introduced, form adventitia, the thickness of described adventitia is 0.02～0.2 μ m.
Owing to having added the transition metal such as Cr and Co, Mo, W, Zr, Ti, Nb, Mn, Ni, the hardness of coating effectively improves, and owing to forming the protective layer (Al of one deck densification after Al oxidation on top layer
100-xm
x)
2o
3thereby, strengthened the corrosion resistance characteristic of Nd-Fe-B magnet, thereby reached the object of protection magnet.
According to a further aspect in the invention, the invention provides the manufacture method with good Anticorrosive Character and harder neodymium iron boron aluminum base alloy coating, described method comprises the steps:
(1) Nd-Fe-B magnet is plated to pre-treatment, treatment process comprises cleaning, the conventional plating pre-processing technique of chamfering;
(2) melting Al base alloy and make needed shape to adopt evaporation process or sputtering technology is processed;
(3) adopt evaporation process or sputtering technology Al base alloy to be plated to the surface of Nd-Fe-B magnet, obtain Al base alloy layer; Or Al with add the surface that metal M is splashed to respectively magnet, then by heat treating method, obtain Al base alloy layer.
(4) described Al base alloy layer obtains the Al base alloy layer with adventitia after top layer Passivation Treatment or top layer oxide treatment.
Wherein, the component of described Al base alloy layer is Al
100-x-M
x, described adventitia is (Al by component
100-x-M
x)
2o
3form; Wherein, M comprises Cr, Co, Mo, W, Zr, Ti, Nb, one or more elements in Mn element; 0.05≤x≤10, x is average atom per-cent.The thickness of described Al base alloy layer is respectively 5～30 μ m, and the thickness of described adventitia is 0.02～0.2 μ m.
Preferably, described heat treated temperature is 300～600 ℃, and soaking time is at least 5～10 minutes.
Preferably, the time of described surface passivating treatment is 5～30 minutes.
Preferably, the temperature of described top layer oxide treatment is 200～400 ℃,
Preferably, the treatment time of described top layer oxide treatment is 30～60 minutes.
The thickness of coating that the present invention obtains is about 5-30 μ m magnet, can be through tens of time mutual collision frictions between magnet and top layer is not damaged, at 5%NaCl, accelerate under the experiment condition of salt fog, magnet Al alloy layer can withstand 96～144 hours, and 5% salt fog accelerates experiment and is not damaged.Under the experiment condition of 100% humidity, 125 celsius temperatures, there is time to rupture 500～1200 hours in can the reach a high temperature PCT experiment of the Al alloy layer of magnet.Use the magnet of Al alloy layer after collision for several times, before finished product packing, under 20 power microscopes, viewed cut per-cent significantly reduces.
Accompanying drawing explanation
Fig. 1 is the sintered nd-fe-b magnet photo in kind after PVD plating Al base alloy;
Fig. 2 is the plating Al magnet photo after the 5%NaCl acceleration salt mist experiment of 144 hours;
Fig. 3 is through 100% humidity, 125 celsius temperatures, the magnet photo after the PCT experiment of 700 hours;
Fig. 4 is plating Al layer cross section metallograph.
Embodiment
By following examples, the present invention is further described in detail, but is not limited in the process parameters range in following examples and embodiment.
Embodiment 1～9
Vacuum melting atomic percent is Al
99.95m
0.05al base alloy, wherein M is respectively a kind of in Cr, Co, Mo, W, Zr, Ti, Nb, Mn, Ni element.Alloy is made to the size and dimension mating with equipment.Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, heating electrode makes the evaporation of Al base alloy, after 1 hour, plates respectively the Al base alloy layer of one deck approximately 5 μ m in Nd-Fe-B magnet surface.Taking out, put into the passivating solution passivation that configures through the magnet of evaporation 5 minutes.After passivation, coating outermost layer forms one deck (Al100-xMx) 2O3 thin layer, and thickness is about 0.02 μ m.The corrosion resistance characteristic that Al base alloy layer is corresponding and surface tear situation refer to table 1.
Embodiment 19～26
Vacuum melting atomic percent is Al
99.95m
0.05al base alloy, wherein M is respectively a kind of in Cr, Co, Mo, W, Zr, Ti, Nb, Mn, Ni element.Alloy is made to the size and dimension mating with equipment.Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, heating electrode makes the evaporation of Al base alloy, after 3 hours, plates respectively the Al base alloy layer of one deck approximately 30 μ m in Nd-Fe-B magnet surface.Taking out, put into the passivating solution passivation that configures through the magnet of evaporation 30 minutes.After passivation, coating outermost layer forms one deck (Al
100-xm
x)
2o
3thin layer, thickness is about 0.2 μ m.The corrosion resistance characteristic that Al base alloy layer is corresponding and surface tear situation refer to table 1.
Embodiment 27～33
Vacuum melting atomic percent is Al
99.95m
0.05al base alloy, wherein M is respectively a kind of in Cr, Co, Mo, W, Zr, Ti, Nb, Mn, Ni element.Alloy is made to the size and dimension mating with equipment.Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, heating electrode makes the evaporation of Al base alloy, after 2 hours, plates respectively the Al base alloy layer of one deck approximately 20 μ m in Nd-Fe-B magnet surface.Taking out, put into the passivating solution passivation that configures through the magnet of evaporation 20 minutes.After passivation, coating outermost layer forms one deck (Al
100-xm
x)
2o
3thin layer, thickness is about 0.1 μ m.The corrosion resistance characteristic that coating is corresponding and surface tear situation refer to table 1.
Embodiment 34～41
Vacuum melting atomic percent is Al
95m
5al base alloy, wherein M is respectively a kind of in Cr, Co, Mo, W, Zr, Ti, Nb, Mn, Ni element.Alloy is made to the size and dimension mating with equipment.Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, heating electrode makes the evaporation of Al base alloy, and after 2 hours, Nd-Fe-B magnet surface plates the Al base alloy layer of one deck approximately 20 μ m respectively.Taking out, put into the passivating solution passivation that configures through the magnet of evaporation 15 minutes.After passivation, coating outermost layer forms one deck (Al
100-xm
x)
2o
3thin layer, thickness is 0.1 μ m left and right.The corrosion resistance characteristic that coating is corresponding and surface tear situation refer to table 1.
Embodiment 42～53
Vacuum melting atomic percent is Al
99m
1al base alloy, wherein M is respectively a kind of alloy in Cr, Co, Mo, W, Zr, Ti, Nb, Mn, Ni element.Alloy is made to the size and dimension mating with equipment.Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, heating electrode makes the evaporation of Al base alloy, and after 2 hours, Nd-Fe-B magnet surface plates the Al base alloy layer of one deck approximately 20 μ m respectively.Taking out, put into the passivating solution passivation that configures through the magnet of evaporation 15 minutes.After passivation, coating outermost layer forms one deck (Al
100-xm
x)
2o
3thin layer, thickness is 0.1 μ m.The corrosion resistance characteristic that coating is corresponding and surface tear situation refer to table 1.
Embodiment 54～61
Vacuum melting atomic percent is Al
99cr
0.5m
0.5al base alloy, wherein M is respectively a kind of in Co, Mo, W, Zr, Ti, Nb, Mn, Ni element.Alloy is made to the size and dimension mating with equipment.Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, heating electrode makes the evaporation of Al base alloy, and after 1.5 hours, Nd-Fe-B magnet surface plates the Al base alloy layer of one deck approximately 18 μ m respectively.Magnet through evaporation is taken out, be placed in air and be heated to 200 ℃ of left and right, keep carrying out for 30 minutes top layer passivation.After oxidation, coating outermost layer forms one deck (Al
100-xm
x)
2o
3thin layer, thickness is 0.02 μ m.The corrosion resistance characteristic that coating is corresponding and surface tear situation refer to table 1.
Embodiment 62
Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, adopt the method for sputter, Al with add metal according to Al
99.5cr
0.5composition ratio is plated to respectively the surface of Nd-Fe-B magnet.According to equipment different situations thickness of coating, be controlled at 25 μ m.Magnet after sputter is put into vacuum oven, be heated to 300 ℃, be incubated 5 hours, obtain required coating.Coating outermost layer after 400 degrees Celsius of oxide treatment of 60 minutes has the zone of oxidation of about 0.2 μ m thickness, and the composition of zone of oxidation alloy is (Al
100-xm
x)
2o
3.The corrosion resistance characteristic that coating is corresponding and surface tear situation refer to table 1.
Embodiment 63～69
Nd-Fe-B sintered magnet is cut into needed size and dimension, through washing, rinse after washing and put into vacuum oven, be evacuated down to 10
-3after Pa, turn off vacuum unit, adopt the method for sputter, Al with add metal according to Al
99.8cr
0.1m
0.1al base alloy, wherein M is respectively a kind of in Co, Mo, W, Zr, Ti, Nb, Mn, Ni element, this Al base alloy is plated to respectively to the surface of Nd-Fe-B magnet.According to equipment different situations thickness of coating, be controlled at 10 μ m.Magnet after sputter is put into vacuum oven, be heated to 300 ℃ of degree, be incubated 5 hours, obtain required coating.The magnet obtaining is taken out, be placed in air and be heated to 300 ℃ of left and right, keep carrying out for 45 minutes top layer passivation.Outermost layer after coating oxidation has the zone of oxidation of about 0.1 μ m thickness, and the composition of zone of oxidation alloy is (Al
100-xm
x)
2o
3.The corrosion resistance characteristic that Al base alloy layer is corresponding and surface tear situation refer to table 1.
Table 1 thickness is corrosion resistance characteristic and the surface tear situation that the Al base alloy layer of 20 μ m is corresponding
As can be seen from Table 1: the thickness of coating obtaining for the present invention is 20 μ m magnets, 1, at 5%NaCl, accelerate under the experiment condition of salt fog, magnet Al alloy layer can withstand 96～144 hours, and 5% salt fog accelerates experiment and is not damaged.2,, under the experiment condition of 100% humidity, 125 celsius temperatures, there is time to rupture 500～1200 hours in can the reach a high temperature PCT experiment of the Al alloy layer of magnet.3, use the magnet of Al alloy layer after collision for several times, before finished product packing, under 20 power microscopes, viewed cut per-cent significantly reduces.This shows the in the situation that of same use physical gas-phase deposite method, the Corrosion Protection of the magnet coating that plating Al alloy of the present invention obtains is suitable with the coating that the pure Al of plating obtains, the Corrosion Protection of Al alloy layer that adds two or more metals is stronger, and use the coating hardness that Al Alloy Plating of the present invention obtains all to strengthen to some extent, thereby can effectively prevent from occurring that cut destroys the situation generation of corrosion resistance nature in manufacture and use procedure.
The present invention is illustrated by embodiment above, and still, the present invention is not limited to particular example as described herein and embodiment.Any those of skill in the art are easy to be further improved without departing from the spirit and scope of the present invention and perfect, therefore the present invention is only subject to the restriction of content and the scope of the claims in the present invention, and its intention contains all alternatives and equivalents that are included in the spirit and scope of the invention being limited by appendix claim.
Claims (10)
1. an aluminum base alloy coating with good Anticorrosive Character and harder neodymium iron boron, the component of described aluminum base alloy coating is Al
100-x-Mx; Wherein, M is Co, Mo, W, Zr, Ti, Nb, and one or more elements in Mn element, or M is Cr and is selected from Co, Mo, W, Zr, Ti, Nb, a kind of element in Mn element; 0.05≤x≤10, x is average atom per-cent.
2. neodymium iron boron aluminum base alloy coating as claimed in claim 1, wherein, the thickness of described aluminum base alloy coating is respectively 5～30 μ m.
3. neodymium iron boron aluminum base alloy coating as claimed in claim 1 or 2, wherein, described aluminum base alloy coating also comprises an adventitia, described adventitia is (Al by component
100-x-M
x)
2o
3form, wherein, M comprises Cr, Co, Mo, W, Zr, Ti, Nb, one or more elements in Mn element; 0.05≤x≤10, x is average atom per-cent.
4. neodymium iron boron aluminum base alloy coating as claimed in claim 3, wherein, the thickness of described adventitia is 0.02～0.2 μ m.
5. a manufacture method with good Anticorrosive Character and harder neodymium iron boron aluminum base alloy coating, described method comprises the steps:
(1) Nd-Fe-B magnet is plated to pre-treatment, treatment process comprises cleaning, the conventional plating pre-processing technique of chamfering;
(2) melting Al base alloy and make needed shape to adopt evaporation process or sputtering technology is processed;
(3) adopt evaporation process or sputtering technology Al base alloy to be plated to the surface of Nd-Fe-B magnet, obtain Al base alloy layer; Or Al with add the surface that metal M is splashed to respectively magnet, then by heat treating method, obtain Al base alloy layer;
(4) described Al base alloy layer obtains the Al base alloy layer with adventitia after top layer Passivation Treatment or top layer oxide treatment;
Wherein, the component of described Al base alloy layer is Al
100-x-M
x, described adventitia is (Al by component
100-x-M
x)
2o
3form; Wherein, M is Co, Mo, W, Zr, Ti, Nb, and one or more elements in Mn element, or M is Cr and is selected from Co, Mo, W, Zr, Ti, Nb, a kind of element in Mn element; 0.05≤x≤10, x is average atom per-cent.
6. manufacture method as claimed in claim 5, wherein, the thickness of described Al base alloy layer is respectively 5～30 μ m, and the thickness of described adventitia is 0.02～0.2 μ m.
7. manufacture method as claimed in claim 5, wherein, described heat treated temperature is 300～600 ℃, soaking time is at least 5～10 minutes.
8. manufacture method as claimed in claim 5, wherein, the time of described surface passivating treatment is 5～30 minutes.
9. manufacture method as claimed in claim 5, wherein, the temperature of described top layer oxide treatment is 200～400 ℃.
10. manufacture method as claimed in claim 5, wherein, the treatment time of described top layer oxide treatment is 30～60 minutes.
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| CN102864430A (en) * | 2012-09-10 | 2013-01-09 | 虞雪君 | Antisepsis method used for neodymium iron boron ferrite surface |
| CN104651782B (en) * | 2013-11-18 | 2018-08-31 | 北京中科三环高技术股份有限公司 | Magnet surface processing method and Sintered NdFeB magnet |
| CN104480475A (en) * | 2014-11-04 | 2015-04-01 | 烟台首钢磁性材料股份有限公司 | Neodymium-iron-boron magnet surface hard aluminum film layer preparation method |
| EP3337912A4 (en) * | 2015-08-20 | 2019-02-20 | Xtalic Corporation | Magnets including an aluminum manganese alloy coating layer and related methods |
| CN105420669B (en) * | 2015-11-29 | 2018-02-02 | 中国人民解放军装甲兵工程学院 | A kind of CVD method for permanent magnet anti-corrosion pre-treatment |
| CN106198366A (en) * | 2016-06-23 | 2016-12-07 | 宁波国际材料基因工程研究院有限公司 | A kind of screening technique of high flux soft magnetic materials surface anticorrosion layer |
| CN110484887A (en) * | 2019-09-17 | 2019-11-22 | 合肥赉晟科技有限公司 | A kind of rare-earth permanent magnet surface fast vacuum aluminum plating method |
| CN110656315A (en) * | 2019-10-28 | 2020-01-07 | 华南理工大学 | Method for improving coercive force and wear-resistant and corrosion-resistant performance of neodymium iron boron magnet |
| CN110993307B (en) * | 2019-12-23 | 2021-10-29 | 南昌航空大学 | Method for improving coercive force and thermal stability of sintered neodymium-iron-boron magnet |
| CN112176286B (en) * | 2020-09-30 | 2022-07-15 | 福建省长汀金龙稀土有限公司 | Coating, metal magnet with coating and preparation method of coating |
| CN113257508B (en) * | 2021-05-13 | 2023-09-01 | 中钢天源股份有限公司 | Manufacturing method of neodymium iron boron |
| CN114574806A (en) * | 2022-03-02 | 2022-06-03 | 浙江大学 | Rare earth permanent magnet material surface corrosion-resistant coating and preparation method thereof |
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