CN102041506A - Surface treatment method of permanent magnet material - Google Patents
Surface treatment method of permanent magnet material Download PDFInfo
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- CN102041506A CN102041506A CN2009102357455A CN200910235745A CN102041506A CN 102041506 A CN102041506 A CN 102041506A CN 2009102357455 A CN2009102357455 A CN 2009102357455A CN 200910235745 A CN200910235745 A CN 200910235745A CN 102041506 A CN102041506 A CN 102041506A
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Abstract
The invention relates to a surface treatment method of a permanent magnet material. The method comprises the following steps: (1) polishing the permanent magnet material; (2) adding alkaline solution to degrease the permanent magnet material; (3) adding acidic solution to carry out acid pickling on the permanent magnet material so as to remove rust; (4) aluminizing the surface of the permanent magnet material under vacuum; and (5) coating an epoxy resin layer on the aluminium coating of the permanent magnet material through electrophoresis. The permanent magnet material treated by the surface treatment method provided by the invention has good antiseptic performance and can keep antiseptic in 1700 hours in the humid heat test and neutral salt spray test and in 500 hours in the high temperature high pressure test; and the magnetic property of the permanent magnet material is slightly degraded at high temperature, and the high temperature demagnetization of the permanent magnet material is only 0.1-0.5% which is far less than 2-15% in the prior art.
Description
Technical field
The present invention relates to a kind of surface treatment method of permanent magnet material, belong to the field of surface treatment of material.
Background technology
Can application of neodymium iron boron (NdFeB) permanent magnet material in recent years and development be very rapid, be to be related to one of gordian technique that can Nd-Fe-Bo permanent magnet material apply and effectively protect Nd-Fe-Bo permanent magnet material.Nd-Fe-Bo permanent magnet material mainly is to be prepared from by powder metallurgical technique by elements such as rare earth metal neodymium, iron and boron.As the strongest present magneticsubstance, be widely used in all fields such as electroplating device, machinery, medical treatment, automobile, application prospect is very wide.
The prerequisite of Nd-Fe-Bo permanent magnet material widespread use is to resolve the anticorrosion problem of Nd-Fe-Bo permanent magnet material.As the porous material that a kind of powder metallurgical technique is prepared from, wherein rich neodymium phase, neodymium iron boron principal phase and borderline phase are easy to form intergranular corrosion.Simultaneously, rear earth element nd in the neodymium iron boron powder alloy, character is active, make the corrosion resisting property of whole Nd-Fe-B alloys become very poor, very easily corrosion in damp and hot environment, because of corrosion failure causes the decline or the damage of magnetic property, had a strong impact on the work-ing life of Nd-Fe-B permanent magnet, reduced the stability and the reliability of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its weave construction have very big relation, and wherein, the principal phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property, and the coercitive relatively contribution of rich neodymium is maximum.After Nd-Fe-Bo permanent magnet material corrodes, the magnetic property of material will be greatly weakened.Therefore, the anticorrosion problem of Nd-Fe-Bo permanent magnet material is to need one of subject matter that solves always.
The anti-corrosion method of Nd-Fe-Bo permanent magnet material has much at present.Electronickelling, electro-galvanizing (CN1421547A, CN1056133A) are wherein arranged, electroplate MULTI-LAYER NICKEL, copper facing (CN1514889A), several different methods such as phosphatization, electrocoating paint.
Publication number provides a kind of corrosion-resisting permanent magnet and manufacture method thereof for the patent of invention of SUMITOMO CHEMICAL Special Metal Co., Ltd. application of CN1272212, plate Al or the Ti film that thickness is 0.06～30 μ m by the rare earth permanent magnet surface of method after cleaning such as ion plating, ion sputtering or physical vapor deposition and chemical vapour depositions, and then feed single O
2Perhaps content is at the O more than 10%
2To form thickness is the amorphous nickel/phosphorus/aluminium oxide rete of 0.1～10 μ m.Improved the erosion resistance of magnet by this method.Permanent magnet is through after the above-mentioned processing, under the condition of 80 ℃ of temperature, relative humidity 90%, can reach in the 1000h and is not corroded.But the result of the neutral salt spray test of the permanent magnet after this surface treatment of process is unsatisfactory.
Simultaneously, the permanent magnet high temperature demagnetize phenomenon after the prior art surface treatment all compares seriously.High temperature demagnetize experimental working technique is with after film forming Nd-Fe-Bo permanent magnet material has been surveyed magnetic flux, at 150 ℃, places and cools to normal temperature after 1 hour, after such 2～3 times, surveys the flux value of Nd-Fe-Bo permanent magnet material again.The variation per-cent of this twice flux value is exactly the high temperature demagnetizing factor.The high temperature demagnetizing factor of prior art is generally 2%～15%.
Summary of the invention
The objective of the invention is in order to overcome the defective of prior art, a kind of not only salt spray resistance but also moisture-proof heat are provided, and can reduce the surface treatment method of the permanent magnet material of high temperature demagnetizing factor.
According to an aspect of the present invention, the surface treatment method that the invention provides a kind of permanent magnet material comprises the steps:
(1) material polishing: described permanent magnet material is polished;
(2) degreasing degreasing: add basic solution grinded permanent magnet material is carried out degreasing degreasing;
(3) acid pickling and rust removing: add the permanent magnet material of acidic solution after and carry out acid pickling and rust removing to degreasing degreasing;
(4) vacuum aluminum-coated: the permanent magnetic material surface after pickling carries out vacuum aluminum-coated formation aluminium coated;
(5) electrophoresis epoxy-based lacquers: by electrophoresis coating epoxy resin layer on the aluminium coated of permanent magnet material.
Preferably, in step (4), adopt vacuum evaporation, vacuum sputtering plating or the permanent magnetic material surface of multi-arc ion coating after pickling to carry out vacuum aluminum-coated; Further preferably, described vacuum evaporation is vacuum arc, vacuum electron beam or vacuum resistance evaporation, and described vacuum sputtering plating is the plating of intermediate frequency magnetically controlled DC sputtering; Described multi-arc ion coating is the rotary magnetron multi-arc ion coating.
Preferably, be ability cathode electrophoresis at electrophoresis described in the step (5), described epoxy resin layer is not leaded; Further preferably, the described epoxy resin layer miscellany that is epoxy polyamide and urethane.
Preferably, be 0.2～10 μ m at the thickness of aluminium coated described in the step (4), the grain size of aluminium is 20～200nm in the described aluminium coated; Further preferably, the thickness of described aluminium coated is 0.5～5 μ m, and the grain size of aluminium is 50～100nm in the described aluminium coated.
Preferably, the thickness of described epoxy resin layer is 10～40 μ m; Further preferably, the thickness of described epoxy resin layer is 20～30 μ m.
Preferably, described permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
Preferably, in step (1), permanent magnet material is polished by mechanical vibration or barreling chamfering method.
Preferably, be sodium phosphate, yellow soda ash or sodium hydroxide solution at basic solution described in the step (1), described acidic solution is a nitric acid.
In the present invention, along with the increase of the thickness of aluminium coated and epoxy resin layer, the Corrosion Protection of permanent magnet material also increases thereupon.But the thickness of aluminium coated and epoxy resin layer neither be the bigger the better, because can increase cost like this, as long as reach etch-proof purpose.Therefore, as preferred embodiment, aluminium coated is no more than 10 μ m, and the thickness of epoxy resin layer is no more than 40 μ m.
Polishing in the surface treatment method of permanent magnet material provided by the present invention, degreasing degreasing and acid pickling and rust removing all belong to this area cleaning surfaces technology commonly used.Can use this area any technique means commonly used to reach the purpose of clean surface.For example, basic solution used in the present invention is selected from one or more in sodium radio-phosphate,P-32 solution, sodium carbonate solution, sodium hydrogen carbonate solution, sodium hydroxide solution or the potassium hydroxide solution, but still have other basic solution of not enumerating, can be used for the technology degreasing degreasing equally., existing basic solution different iff being to use carries out degreasing degreasing, then just to the simple replacement of technical characterictic of the present invention.
Vacuum aluminum-coated technology in the surface treatment method of permanent magnet material provided by the present invention and electrophoresis coating Resins, epoxy technology all belong to technology commonly used in this area, and inventive point of the present invention mainly is above-mentioned two kinds of technology are combined, and carry out earlier vacuum aluminum-coated, after carry out electrophoresis coating Resins, epoxy.Therefore, for example, only adopting certain technology of aluminizing commonly used of this area to replace the cited vacuum evaporation of the present invention, vacuum sputtering plating or multi-arc ion coating, then is the simple replacement to technical characterictic of the present invention.
The surface treatment method of permanent magnet material provided by the present invention compared with prior art, has following beneficial effect:
1, the permanent magnetic material surface after surface treatment method provided by the invention is handled is even, have good Corrosion Protection: humid heat test (80 ℃ of temperature, relative humidity 90%) and neutral salt spray test all can reach 1700 hours, and high temperature and pressure test is 500 hours; 2, the high temperature demagnetizing factor of the permanent magnet material handled of surface treatment method provided by the present invention is very little, only is 0.1%～0.5%, far below the high temperature demagnetizing factor 2%～15% of prior art like product.
Embodiment
For making your auditor can further understand technical scheme of the present invention and purpose thereof, now be described in detail as follows in conjunction with appended preferred embodiment, illustrated preferred embodiment only is used to technical scheme of the present invention is described, and non-limiting the present invention.
Embodiment 1
Earlier with the mechanical vibration 2 hours in vibrating ball mill of the sintered Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg, use basic solution (sodium phosphate 20g/L, yellow soda ash 10g/L and sodium hydroxide 10g/L) degreasing degreasing then, pickling in 1% salpeter solution subsequently, to remove the oxide compound of permanent magnetic material surface, last flushing with clean water, dry up, obtain the permanent magnet material of cleaning surfaces.The method of employing vacuum arc vacuum evaporation is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 10 μ m, and the grain size of aluminium is 200nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 10 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Embodiment 2
According to the method for embodiment 1 binding Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg is carried out cleaning surfaces.The method of employing vacuum electron beam vacuum evaporation is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 0.2 μ m, and the grain size of aluminium is 100nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 30 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Embodiment 3
According to the method for embodiment 1 sintered Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg is carried out cleaning surfaces.The method of employing rotary magnetron multi-arc ion coating is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 0.5 μ m, and the grain size of aluminium is 20nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 40 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Embodiment 4
According to the method for embodiment 1 binding Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg is carried out cleaning surfaces.The method that adopts the intermediate frequency magnetically controlled DC sputtering to plate is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 2 μ m, and the grain size of aluminium is 50nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 20 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Embodiment 5
According to the method for embodiment 1 binding Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg is carried out cleaning surfaces.The method of employing vacuum resistance evaporation is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 100nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 25 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Embodiment 6
According to the method for embodiment 1 binding Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg is carried out cleaning surfaces.The method of employing radio frequency magnetically controlled DC sputtering is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 2 μ m, and the grain size of aluminium is 60nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 30 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Embodiment 7
According to the method for embodiment 1 binding Nd-Fe-B permanent magnetic material of ￠ 24 * ￠ 15 * 18mm of 2.5kg is carried out cleaning surfaces.It is vacuum aluminum-coated to adopt the vacuum cathode multi-arc ion coating to adopt the method for non-magnetic control rotation to carry out on the permanent magnet material clean Surface, and the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 30nm in the aluminium coated; The ability cathode electrophoresis method coating thickness on the aluminium coated of permanent magnet material that adopts routine is that the epoxy resin layer of 20 μ m is the miscellany of epoxy polyamide and urethane, disposes.
Here it is to be noted, polishing among the embodiment 1～7, degreasing degreasing and acid pickling and rust removing are this area prior art commonly used, and not emphasis of the present invention, therefore embodiment 1～7 adopted that identical method and operational condition are polished, degreasing degreasing and acid pickling and rust removing, this and do not mean that can only polish according to these methods and operational condition, degreasing degreasing and acid pickling and rust removing, but can polish according to any possibility method and operational condition that those skilled in the art knew and knew, degreasing degreasing and acid pickling and rust removing.
The comparative example 1
According to the method for embodiment 1 Nd-Fe-Bo permanent magnet material of ￠ 24 * ￠ 15 * 18mm of 2.3kg is carried out cleaning surfaces.The method of employing vacuum arc vacuum evaporation is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 200nm in the aluminium coated, disposes.
The comparative example 2
According to the method for embodiment 1 Nd-Fe-Bo permanent magnet material of ￠ 24 * ￠ 15 * 18mm of 2.3kg is carried out cleaning surfaces.The method of employing vacuum electron beam vacuum evaporation is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 100nm in the aluminium coated, disposes.
The comparative example 3
According to the method for embodiment 1 Nd-Fe-Bo permanent magnet material of ￠ 24 * ￠ 15 * 18mm of 2.3kg is carried out cleaning surfaces.The method that adopts the intermediate frequency magnetically controlled DC sputtering to plate is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 60nm in the aluminium coated, disposes.
The comparative example 4
According to the method for embodiment 1 Nd-Fe-Bo permanent magnet material of ￠ 24 * ￠ 15 * 18mm of 2.3kg is carried out cleaning surfaces.The method of employing rotary magnetron multi-arc ion coating is carried out vacuum aluminum-coated on the permanent magnet material clean Surface, and the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 100nm in the aluminium coated, disposes.
The comparative example 5
Earlier with the mechanical vibration 2 hours in vibrating ball mill of the Nd-Fe-Bo permanent magnet material of ￠ 24 * ￠ 15 * 18mm of 2.3kg, use basic solution (sodium phosphate 20g/L, yellow soda ash 10g/L and sodium hydroxide 10g/L) degreasing degreasing then, pickling in 1% salpeter solution subsequently, to remove the oxide compound of permanent magnetic material surface, after the flushing with clean water 3 times again the sulphuric acid soln with 5% activate, obtain the permanent magnet material of cleaning surfaces.On the permanent magnet material clean Surface, carry out nickel plating; The ability cathode electrophoresis method coating thickness on the nickel layer of permanent magnet material that adopts routine is that the epoxy resin layer of 40 μ m is the miscellany of epoxy polyamide and urethane, disposes.
The permanent magnet material of embodiment 1～7 and comparative example's 1～5 gained is carried out anti-corrosion performance test and the test of high temperature demagnetize, and with logging in table 1.Wherein, anti-corrosion performance test comprises neutral salt spray test, humid heat test (80 ℃ of temperature, relative humidity 90%) and high temperature and pressure test (be the PCT test, test conditions is PH=12.5,148 ℃, 70Mpa).
Neutral salt spray test carries out according to the method that standard GB 6458-86 goes up record: the sodium chloride aqueous solution with 5% (pH is 6.5～7.2), temperature be 35 ℃ ± 2 ℃, relative humidity greater than 95% condition under, with the certain mist amount of falling [1～2mL/ (80cm
2H)] be sprayed on the passive film, adopt the mode of spraying continuously, every 24h is an one-period.
High temperature demagnetize test is carried out in accordance with the following methods: the magnetic flux of measuring the Nd-Fe-Bo permanent magnet material of handling with surface treatment method provided by the present invention, then this permanent magnet material was placed 1 hour in 150 ℃ environment, cool to normal temperature (20 ℃) subsequently, so handle altogether and carry out repeatedly 3 times, and then the magnetic flux of measurement Nd-Fe-Bo permanent magnet material, by calculating the high temperature demagnetizing factor.
Magnetic flux * 100 of the permanent magnet material before high temperature demagnetizing factor=(magnetic flux of the permanent magnet material after the magnetic flux of the permanent magnet material before the test of high temperature demagnetize-high temperature demagnetize test)/high temperature demagnetize test.
The result of the anti-corrosion performance test of the permanent magnet material of table 1 embodiment 1～7 and comparative example's 1～5 gained and the test of high temperature demagnetize
As can be seen from Table 1, after the method that permanent magnet material is provided according to embodiment 1～7 is carried out surface treatment, has good antiseptic property, not only high temperature and pressure test and humid heat test have reached 500 hours respectively and 1700 hours, and neutral salt spray test also reached 1700 hours, so its antiseptic property is far superior to the corrosion-resisting permanent magnet that patent CN1272212 is provided.And use surface treatment method provided by the present invention to greatly reduce the high temperature demagnetizing factor of permanent magnet material, the high temperature demagnetizing factor of permanent magnet material can be controlled at below 0.5% high temperature demagnetizing factor far below of the prior art 2～15%.
1～4 of comparative example has carried out cleaning surfaces to permanent magnet material and has handled and aluminize, and wherein, the thickness of aluminium coated is 5 μ m, and the grain size of aluminium is 60～200nm in the aluminium coated.The thickness of the aluminium coated of the permanent magnet material of embodiment 1～7 is 0.2～10 μ m, and the grain size of aluminium is 20～200nm in the aluminium coated.The aluminium coated of comparative example 1～4 aluminium coated and embodiment 1～7 is basic identical, but it is very big that the antiseptic property of the permanent magnet material of the two differs, the high temperature and pressure test and the humid heat test of the permanent magnet material of comparative example's 1～4 gained are 48 hours, and neutral salt spray test only is 8 hours, can not reach relevant national standard.
Comparative example 5 carries out cleaning surfaces to permanent magnet material earlier and handles, and its cleaning surfaces is handled different with above-mentioned each embodiment, not only comprise polishing, degreasing degreasing and acid pickling step, but also useful sulfuric acid carries out the step of surface active; Then permanent magnet material is carried out nickel plating and electrophoresis coating Resins, epoxy.Test the test of Corrosion Protection with the permanent magnet material of comparative example's 5 gained, its high temperature and pressure test, humid heat test and neutral salt spray test were respectively 24 hours, 200 hours and 200 hours.This shows that the antiseptic property of the permanent magnet material of comparative example's 5 gained is better than the antiseptic property of comparative example's 1～4 gained permanent magnet material, but be inferior to the antiseptic property of the permanent magnet material of embodiment 1～7 gained far away.Simultaneously, another defective of the method that comparative example 5 is provided is to have bigger high temperature demagnetizing factor (8%) through the permanent magnet material that this method is handled, and is more than 16 times of high temperature demagnetizing factor of the permanent magnet material of embodiment 1～7 gained.
From embodiment 1～7 and comparative example's 1～5 comparison, as can be seen, has only the effect that aluminium coated and epoxy resin layer are combined and just can play protection against corrosion and reduce the high temperature demagnetizing factor.As a kind of preferred implementation of the present invention, use and do not contain plumbous Resins, epoxy electrophoresis coating permanent magnet material, resulting permanent magnet material not only has above-described various advantage, but also has the advantage of environmental protection.
Need to prove that foregoing invention content and embodiment are intended to prove the practical application of technical scheme provided by the present invention, should not be construed as qualification protection domain of the present invention.Those skilled in the art are in spirit of the present invention and principle, when doing various modifications, being equal to and replacing 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 is characterized in that, described surface treatment method comprises the steps:
(1) material polishing: described permanent magnet material is polished;
(2) degreasing degreasing: add basic solution grinded permanent magnet material is carried out degreasing degreasing;
(3) acid pickling and rust removing: add the permanent magnet material of acidic solution after and carry out acid pickling and rust removing to degreasing degreasing;
(4) vacuum aluminum-coated: the permanent magnetic material surface after pickling carries out vacuum aluminum-coated formation aluminium coated;
(5) electrophoresis epoxy-based lacquers: by electrophoresis coating epoxy resin layer on the aluminium coated of permanent magnet material.
2. surface treatment method according to claim 1 is characterized in that, adopts vacuum evaporation, vacuum sputtering plating or the permanent magnetic material surface of multi-arc ion coating after pickling to carry out vacuum aluminum-coated in step (4).
3. surface treatment method according to claim 2 is characterized in that, described vacuum evaporation is vacuum arc, vacuum electron beam or vacuum resistance evaporation; Described vacuum sputtering plating is the plating of intermediate frequency magnetically controlled DC sputtering; Described multi-arc ion coating is the rotary magnetron multi-arc ion coating.
4. surface treatment method according to claim 1 is characterized in that, is ability cathode electrophoresis at electrophoresis described in the step (5), and described epoxy resin layer is not leaded.
5. according to claim 1 or 4 described surface treatment methods, it is characterized in that described epoxy resin layer is the miscellany of epoxy polyamide and urethane.
6. surface treatment method according to claim 1 is characterized in that, is 0.2～10 μ m at the thickness of aluminium coated described in the step (4), and the grain size of aluminium is 20～200nm in the described aluminium coated.
7. surface treatment method according to claim 6 is characterized in that, the thickness of described aluminium coated is 0.5～5 μ m, and the grain size of aluminium is 50～100nm in the described aluminium coated.
8. surface treatment method according to claim 5 is characterized in that, the thickness of epoxy resin layer described in the step (5) is 10～40 μ m.
9. surface treatment method according to claim 8 is characterized in that, the thickness of described epoxy resin layer is 20～30 μ m.
10. surface treatment method according to claim 1 is characterized 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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| CN107653440A (en) * | 2017-09-26 | 2018-02-02 | 湖北汽车工业学院 | A kind of method that sintered Nd-Fe-B permanent magnet surface prepares aluminium or mock silver coating |
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