CN102400189A - Surface treatment method for neodymium iron boron permanent magnetic material by organic aluminum plating - Google Patents
Surface treatment method for neodymium iron boron permanent magnetic material by organic aluminum plating Download PDFInfo
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- CN102400189A CN102400189A CN2010102800323A CN201010280032A CN102400189A CN 102400189 A CN102400189 A CN 102400189A CN 2010102800323 A CN2010102800323 A CN 2010102800323A CN 201010280032 A CN201010280032 A CN 201010280032A CN 102400189 A CN102400189 A CN 102400189A
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Abstract
The present invention provides an organic aluminum plating method for a neodymium iron boron permanent magnetic material. The method comprises the following steps: (1) carrying out chamfering and polishing; (2) carrying out degreasing and deoiling; (3) carrying out pickling and derusting; (4) carrying out organic aluminum plating: adopting an aluminum plating solution to carry out aluminum layer plating on the surface of the neodymium iron boron permanent magnetic material under the protection of inert gas, wherein the aluminum plating solution comprises AlCl3, LiAlH4 and tetrahydrofuran; (5) passivating the aluminum plating layer. With the organic aluminum plating method of the present invention, the neodymium iron boron permanent magnetic material can have the excellent corrosion resistance.
Description
Technical field
The present invention relates to a kind of surface treatment method of Nd-Fe-Bo permanent magnet material, particularly a kind of organic aluminized surface treatment method of Nd-Fe-Bo permanent magnet material
Background technology
Application of neodymium iron boron (NdFeB) permanent magnet material in recent years and development very rapidly, and the protection of Nd-Fe-Bo permanent magnet material is to be related to one of gordian technique that can Nd-Fe-Bo permanent magnet material apply.Nd-Fe-Bo permanent magnet material mainly is prepared from through powder metallurgical technique elements such as rare earth metal neodymium (Nd), iron and boron.As the strongest present magneticsubstance, Nd-Fe-Bo permanent magnet material has been widely used in fields such as electroplating device, machinery, medical treatment, automobile, and application prospect is very wide.
The prerequisite that Nd-Fe-Bo permanent magnet material is used is at first to resolve the anticorrosion problem of Nd-Fe-Bo permanent magnet material.As a kind of porous material that is prepared from powder metallurgical technique, rich neodymium phase, neodymium iron boron principal phase and borderline phase in the Nd-Fe-Bo permanent magnet material are easy to form intergranular corrosion.Because the character of the rear earth element nd in the neodymium iron boron powder alloy is active; Thereby the corrosion resisting property that makes whole Nd-Fe-B alloys becomes very poor; Particularly very easily corrosion in damp and hot environment; And, had a strong impact on the work-ing life of Nd-Fe-Bo permanent magnet material because of corrosion failure causes the decline or the damage of magnetic property, reduced the stability and the safety of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its weave construction have very big relation.The principal phase of Nd-Fe-Bo permanent magnet material is the main source of its magnetic property, and to coercive force contribution maximum be rich neodymium phase.After Nd-Fe-Bo permanent magnet material corrodes, huge variation will take place in its magnetic property.Therefore, the anticorrosion problem of Nd-Fe-Bo permanent magnet material is the subject matter that Nd-Fe-Bo permanent magnet material need solve always.
At present, the anti-corrosion method of Nd-Fe-Bo permanent magnet material has a variety of, for example electronickelling, electro-galvanizing (CN1421547A, CN1056133A), plating MULTI-LAYER NICKEL, copper facing (CN1514889A), phosphatization, electrocoating paint etc.
Application number is the organic solution that 200510018865.1 Chinese invention patent application discloses a kind of Nd-Fe-B rare earth permanent magnetic material Electroplating Aluminum, and this organic solution is made up of organic salt, aluminum halide, organic additive and inorganic additives.Through using this organic solution Electroplating Aluminum, can obtain purity and reach 99.9% silvery white, the fine and close aluminium metal coating of light.This aluminium metal coating and matrix bond are good, and neutral salt spray test can reach 200 hours.But be to use this organic solution Electroplating Aluminum to have the problem of cost height, bad maintenance.
Summary of the invention
The object of the present invention is to provide a kind of organic aluminized surface treatment method of Nd-Fe-Bo permanent magnet material, said method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: use sodium phosphate, yellow soda ash or sodium hydroxide to carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that said Nd-Fe-Bo permanent magnet material is carried out the absolute ethyl alcohol of conventional acid pickling and rust removing, washing, adding SODIUM SULPHATE ANHYDROUS 99PCT then, put into THF;
(4) organic aluminizing: go in the groove said Nd-Fe-Bo permanent magnet material is charged, under protection of inert gas, use the liquid of aluminizing that neodymium-iron-boron permanent magnetic material surface is carried out aluminium coated; Wherein, said aluminium liquid comprises AlCl
3, LiAlH
4And THF; With
(5) be heating and curing, with passivation, sealing aluminium coated.
Preferably, the concentration of said aluminium liquid is 0.7～1.3mol/L.AlCl in the said aluminium liquid
3And LiAlH
4Mol ratio be 1～3: 1, the consumption of THF be the 850-950 milliliter/liter.
Preferably, use the absolute ethyl alcohol of SODIUM SULPHATE ANHYDROUS 99PCT to wash said Nd-Fe-Bo permanent magnet material at least three times.
Preferably, said rare gas element is nitrogen or argon gas.
Preferably, the thickness of said aluminium coated is the 5-30 micron, and the size of the crystal grain of said aluminium coated is the 20-200 nanometer.
Preferably, said Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
In organic aluminized method of the present invention, at first Nd-Fe-Bo permanent magnet material is carried out surface treatment, this surface treatment can adopt currently known methods of the prior art to carry out.For example, at first use mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is polished.Use basic soln that Nd-Fe-Bo permanent magnet material is carried out degreasing degreasing then, for example Nd-Fe-Bo permanent magnet material is put into the basic soln that sodium hydroxide that the sodium phosphate that risen by 20g/, yellow soda ash that 10g/ rises and 10g/ rise forms and carry out degreasing degreasing.Then this Nd-Fe-Bo permanent magnet material is carried out acid pickling and rust removing, for example use the salpeter solution of 1% (volume ratio) to clean the oxide compound of removing this neodymium-iron-boron permanent magnetic material surface.Final rinse water falls the acid and the impurity of neodymium-iron-boron permanent magnetic material surface.And in organic aluminized method of the present invention, can adopt any method passivation aluminium coat of the prior art.
Organic aluminum plating method operation of the present invention is simple relatively, and employed plating bath has lower volatility and inflammableness, and can not produce corrosion to body material.Simultaneously, the working temperature of organic aluminum plating process of the present invention is low, thereby has reduced energy consumption, reduced cost, and can not influence the mechanical property of body material (Nd-Fe-Bo permanent magnet material).
Organic aluminum plating method of the application of the invention can plate the aluminium coat of one deck high purity (99.99%) on the surface of Nd-Fe-Bo permanent magnet material, and this aluminium coat quality is good, porosity is low, and does not have the hydrogen embrittlement phenomenon., can improve this aluminium coat the antiseptic property of Nd-Fe-Bo permanent magnet material after being carried out passivation effectively.
Embodiment
In order further to understand structure of the present invention, characteristic and other purposes, combine appended preferred embodiment to specify as follows at present, illustrated preferred embodiment only is used to technical scheme of the present invention is described, and non-limiting the present invention.
Embodiment 1
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid; The absolute ethyl alcohol that is added with SODIUM SULPHATE ANHYDROUS 99PCT is crossed in washing,, put into THF; Under argon shield, aluminize current density 0.5A/ square decimeter.The composition of said aluminium liquid is 0.7mol/L, AlCl
3: LiAlH
4Mol ratio be 1: 1, with 0.7mol AlCl
3With 950 milliliters of LiAlH
4With the THF is 1 liter of solvent Rongcheng.5 microns of aluminum layer thickness, aluminium grain size 20 nanometers in the aluminium lamination.Product water after electroplating was successively carried out alumilite process 60 minutes in 15% sulfuric acid, and electric current 2 peace/square decimeters use 10% SRM 935a 92 ℃ of sealings again after the washing, dry up.Carry out salt-fog test, PCT test and humid heat test then, do not rise through coating and peel off, non-scale, bonding force is fine, and Corrosion Protection is referring to table 1.
Embodiment 2
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid; The absolute ethyl alcohol that is added with SODIUM SULPHATE ANHYDROUS 99PCT is crossed in washing, cleans through three absolute ethyl alcohols; Under nitrogen protection, Electroplating Aluminum, current density 2A/ square decimeter.The composition of said aluminium liquid is 1.3mol/L, AlCl
3: LiAlH
4Mol ratio be 3: 1, all the other are 850 milliliters/liter of THFs.30 microns of aluminum layer thickness, aluminium lamination aluminium grain size 200 nanometers.Product water after electroplating was successively carried out alumilite process 60 minutes in 15% sulfuric acid, and electric current goes out the 2A/ square decimeter, seals 20 fens at 92 ℃ with 10% SRM 935a after the washing again, dries up.Carry out salt-fog test, PCT test and humid heat test then, do not rise through coating and peel off, non-scale, bonding force is fine, and Corrosion Protection is referring to table 1.
Embodiment 3
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter is after sodium hydroxide 10g/ rises degreasing degreasing; Oxide on surface is removed in pickling in 1% nitric acid, and the absolute ethyl alcohol that is added with SODIUM SULPHATE ANHYDROUS 99PCT is crossed in washing; Clean through three absolute ethyl alcohols, put into THF, again; Under argon shield, Electroplating Aluminum, current density 1.5A/ square decimeter.The composition of said aluminium liquid is 1.2mol/L, and AlCl3 is 2 to the mol ratio of LiAlH4, and all the other are 900 milliliters/liter of THFs.10 microns of aluminum layer thickness, aluminium grain size 120 nanometers.Product water after electroplating is successively carried out alumilite process in 15% sulfuric acid, use 10% SRM 935a again, dry up 92 ℃ of sealings.Product water after electroplating was successively carried out alumilite process 60 minutes in 15% sulfuric acid, and electric current goes out the 2A/ square decimeter, seals 20 fens at 92 ℃ with 10% SRM 935a after the washing again, dries up.Carry out salt-fog test, PCT test and humid heat test then, do not rise through coating and peel off, non-scale, bonding force is fine, and Corrosion Protection is referring to table 1.
Embodiment 4
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter is after sodium hydroxide 10g/ rises degreasing degreasing; Oxide on surface is removed in pickling in 1% nitric acid, and the absolute ethyl alcohol that is added with SODIUM SULPHATE ANHYDROUS 99PCT is crossed in washing; Clean through three absolute ethyl alcohols, put into THF, under nitrogen protection; Electroplating Aluminum, current density 1.2A/ square decimeter.The composition of said aluminium liquid is 1.0mol/L, AlCl
3: LiAlH
4Mol ratio be 2.3: 1, all the other are 880 milliliters/liter of THFs.20 microns of aluminum layer thickness, aluminium grain size 100 nanometers.Product water after electroplating was successively carried out alumilite process 60 minutes in 15% sulfuric acid, and electric current goes out the 2A/ square decimeter, seals 20 fens at 92 ℃ with 10% SRM 935a after the washing again, dries up.Carry out salt-fog test, PCT test and humid heat test then, do not rise through coating and peel off, non-scale, bonding force is fine, and Corrosion Protection is referring to table 1.
Embodiment 5
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter is after sodium hydroxide 10g/ rises degreasing degreasing; Oxide on surface is removed in pickling in 1% nitric acid, and the absolute ethyl alcohol that is added with SODIUM SULPHATE ANHYDROUS 99PCT is crossed in washing; Clean through three absolute ethyl alcohols, put into THF, under argon shield; Electroplating Aluminum, current density 1.2A/ square decimeter.The composition of said aluminium liquid is 0.8mol/L, AlCl
3To LiAlH
4Mol ratio be 1.5, all the other are 860 milliliters/liter of THFs.18 microns of aluminum layer thickness, aluminium grain size 100 nanometers.Product water after electroplating was successively carried out alumilite process 60 minutes in 15% sulfuric acid, and electric current goes out the 2A/ square decimeter, seals 20 fens at 92 ℃ with 10% SRM 935a after the washing again, dries up.Carry out salt-fog test, PCT test and humid heat test then, do not rise through coating and peel off, non-scale, bonding force is fine, and Corrosion Protection is referring to table 1.
Embodiment 6
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter is after sodium hydroxide 10g/ rises degreasing degreasing; Oxide on surface is removed in pickling in 1% nitric acid, and the absolute ethyl alcohol that is added with SODIUM SULPHATE ANHYDROUS 99PCT is crossed in washing; Clean through three absolute ethyl alcohols, put into THF, under nitrogen protection; Electroplating Aluminum, current density 1.1A/ square decimeter.The composition of said aluminium liquid is 1.1mol/L, AlCl
3To LiAlH
4Mol ratio be 1, all the other are 930 milliliters/liter of THFs.25 microns of aluminum layer thickness, aluminium grain size 80 nanometers.Product water after electroplating was successively carried out alumilite process 60 minutes in 15% sulfuric acid, and electric current goes out the 2A/ square decimeter, seals 20 fens at 92 ℃ with 10% SRM 935a after the washing again, dries up.Carry out salt-fog test, PCT test and humid heat test then, do not rise through coating and peel off, non-scale, bonding force is fine, and Corrosion Protection is referring to table 1.
Below, the experimental data of physical parameter is carried out in table 1 explanation through the coating that the foregoing description 1～6 is obtained.
Table 1
| Embodiment | Salt fog (hour) | PCT (hour) | Damp and hot (hour) |
| Embodiment 1 | 72 | 72 | 300 |
| Embodiment 2 | 72 | 72 | 300 |
| Embodiment 3 | 72 | 72 | 300 |
| Embodiment 4 | 72 | 72 | 300 |
| Embodiment 5 | 48 | 72 | 300 |
| Embodiment 6 | 48 | 72 | 300 |
Can find out by table 1, electrolytic coating of the present invention surface evenly, solidity to corrosion is high, the humid heat test (85 ℃ of temperature, humidity 80, relative humidity 100%) and the neutral salt spray test of PCT (high temperature and pressure test) 72 hours and 280 hours have good preservative effect.
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 replacement or improvement.Protection scope of the present invention is as the criterion with appended claims.
Claims (7)
1. the organic aluminized surface treatment method of a Nd-Fe-Bo permanent magnet material, said method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: use sodium phosphate, yellow soda ash or sodium hydroxide to carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that said Nd-Fe-Bo permanent magnet material is carried out the absolute ethyl alcohol of conventional acid pickling and rust removing, washing, adding SODIUM SULPHATE ANHYDROUS 99PCT then, put into THF;
(4) organic aluminizing:, under protection of inert gas, use the liquid of aluminizing that neodymium-iron-boron permanent magnetic material surface is carried out electroplating aluminum coating with said Nd-Fe-Bo permanent magnet material; Wherein, said aluminium liquid comprises AlCl
3, LiAlH
4And THF; With
(5) be heating and curing, with passivation, sealing aluminium coated.
2. method according to claim 1 is characterized in that, the concentration of said aluminium liquid is 0.7～1.3mol/L.
3. method according to claim 1 and 2 is characterized in that, the AlCl in the said aluminium liquid
3And LiAlH
4Mol ratio be 1～3: 1, the consumption of THF be the 850-950 milliliter/liter.
4. method according to claim 1 is characterized in that, uses the absolute ethyl alcohol of SODIUM SULPHATE ANHYDROUS 99PCT to wash said Nd-Fe-Bo permanent magnet material at least three times.
5. method according to claim 1 is characterized in that, said rare gas element is nitrogen or argon gas.
6. method according to claim 1 is characterized in that, the thickness of said aluminium coated is the 5-30 micron, and the size of the crystal grain of said aluminium coated is the 20-200 nanometer.
7. method according to claim 1 is characterized in that, said Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
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| CN102766891A (en) * | 2012-07-18 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Method for electrodepositing Al protective plated layer on surface of NdFeB magnet by using ionic liquid |
| CN103334132A (en) * | 2013-07-17 | 2013-10-02 | 沈阳大学 | Method for preparing aluminum-magnesium alloy membrane through electro-deposition at room temperature |
| CN103710739A (en) * | 2012-10-09 | 2014-04-09 | 南昌航空大学 | Preparation method of sintered neodymium-iron-boron permanent-magnet surface ceramic coating |
| CN104213162A (en) * | 2013-06-04 | 2014-12-17 | 天津三环乐喜新材料有限公司 | Surface treatment method for zinc alloy electroplating of automobile permanent magnetic material |
| 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 |
| CN104651783A (en) * | 2015-02-12 | 2015-05-27 | 烟台首钢磁性材料股份有限公司 | Method for plating aluminum on surface of permanent magnet neodymium iron boron magnetic steel |
| CN110233037A (en) * | 2018-03-05 | 2019-09-13 | 宁波招宝磁业有限公司 | A kind of neodymium iron boron surface infiltration dysprosium technique |
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| CN102766891A (en) * | 2012-07-18 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Method for electrodepositing Al protective plated layer on surface of NdFeB magnet by using ionic liquid |
| CN103710739A (en) * | 2012-10-09 | 2014-04-09 | 南昌航空大学 | Preparation method of sintered neodymium-iron-boron permanent-magnet surface ceramic coating |
| CN103710739B (en) * | 2012-10-09 | 2016-07-13 | 南昌航空大学 | The preparation method of sintered Nd-Fe-B permanent magnet surface ceramic coat |
| CN104213162A (en) * | 2013-06-04 | 2014-12-17 | 天津三环乐喜新材料有限公司 | Surface treatment method for zinc alloy electroplating of automobile permanent magnetic material |
| CN104213162B (en) * | 2013-06-04 | 2018-08-21 | 天津三环乐喜新材料有限公司 | A kind of surface treatment method of automobile permanent magnetic material electroplating kirsite |
| CN103334132A (en) * | 2013-07-17 | 2013-10-02 | 沈阳大学 | Method for preparing aluminum-magnesium alloy membrane through electro-deposition at room temperature |
| CN103334132B (en) * | 2013-07-17 | 2016-05-25 | 沈阳大学 | The method of almag film is prepared in room temperature electro-deposition |
| 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 |
| US10204724B2 (en) | 2014-11-04 | 2019-02-12 | Yantai Shougang Magnetic Materials Inc. | Method of preparing a hard aluminum film on the surface of a Nd-Fe-B magnet |
| CN104651783A (en) * | 2015-02-12 | 2015-05-27 | 烟台首钢磁性材料股份有限公司 | Method for plating aluminum on surface of permanent magnet neodymium iron boron magnetic steel |
| CN110233037A (en) * | 2018-03-05 | 2019-09-13 | 宁波招宝磁业有限公司 | A kind of neodymium iron boron surface infiltration dysprosium technique |
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Application publication date: 20120404 |