CN101029389A - Surface protection of neodymium iron boron permanent-magnet material - Google Patents
Surface protection of neodymium iron boron permanent-magnet material Download PDFInfo
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- CN101029389A CN101029389A CN 200710090596 CN200710090596A CN101029389A CN 101029389 A CN101029389 A CN 101029389A CN 200710090596 CN200710090596 CN 200710090596 CN 200710090596 A CN200710090596 A CN 200710090596A CN 101029389 A CN101029389 A CN 101029389A
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Abstract
A surface protection technology of neodymium-ferrous-boron permanent magnetic material is carried out by grinding for neodymium-ferrous-boron permanent magnetic material, degreasing while removing oil, removing rust while acid cleaning, activating acid liquid, putting it into black liquid or blue liquid, chemically coating and forming into blue-black or dark blue protection film. It has excellent combination and anti-corrosion performances.
Description
Technical field
The present invention relates to field of chemical processing of material, especially relate to the surface protection technique of Nd-Fe-Bo permanent magnet material.
Background technology
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-Bo permanent magnet material is related to one of gordian technique that can material apply.This material mainly is to be prepared from by powder metallurgical technique by elements such as rare earth metal neodymium (Nd), 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 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 the porous material that a kind of powder metallurgical technique is prepared from, because of rich neodymium phase wherein, neodymium iron boron principal phase and borderline phase are easy to form intergranular corrosion.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, cause the decline or the damage of magnetic property because of corrosion failure, have 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.The principal phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property.To coercive force contribution maximum is rich neodymium phase.Huge variation will take place in the magnetic property of material after corrosion takes place Nd-Fe-Bo permanent magnet material.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.
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, several different methods such as phosphatization, electrocoating paint.The main drawback of these methods is:
Electrochemical plating: because Nd-Fe-Bo permanent magnet material is a vesicular structure, plating bath can enter into material internal in electroplating process, causes inner intergranular corrosion; And be difficult to obtain quality coating in material inner wall surface electrochemical plating, and coating life is short.
Electrophoretic method: coat-thickness is inhomogeneous, and the hanging point phenomenon is arranged.
Spraying method: complex process, the equipment requirements height, investment is high, and cost is big.
So, more than these means of defences caused reliability of material decline.
The metallic substance black-emitting technology is used for steel surface (referring to CN1453394) more, and the surface blackening technology that is used for Nd-Fe-Bo permanent magnet material then seldom.Domestic neodymium iron boron black-emitting technology also is in blank now, seldom sees report.Shortcomings such as existing black film is compared with traditional copper selenium black film, and the ubiquity blackness is not good, matt, solidity to corrosion is poor, bonding force is bad can not be fit to industrial requirement.Copper selenium class black film not only costs an arm and a leg but also aftertreatment technology complexity, production cost height, and Working environment is not ideal enough, and its application is restricted.The chemical conversion film that adopts material surface nontoxic or that the non-selenium class of low toxicity hair blackening liquid is handled to obtain superior performance at present is the forward position of domestic and international black film, but the relevant report of employing molybdenum aluminium lamination seldom.On the other hand, how to make black film before formation and can effectively to carry out excellent protection to Nd-Fe-Bo permanent magnet material after forming then be a main problem.After film forming NdFeB material has been surveyed magnetic flux, at 150 ℃, place and cool to normal temperature after 1 hour, after 2-3 time, survey the flux value of Nd-Fe-Bo permanent magnet material more like this.The variation per-cent of this twice flux value is exactly the high temperature demagnetize.The high temperature demagnetize of the material that common technology is done is at 2-15%.
Summary of the invention
Goal of the invention of the present invention for the blank of the black-emitting technology of filling up present neodymium-iron-boron permanent magnetic material surface, provides a kind of new neodymium-iron-boron permanent magnetic material surface means of defence just.
The process for protecting surface of Nd-Fe-Bo permanent magnet material of the present invention comprises the steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that Nd-Fe-Bo permanent magnet material is polished;
(2) degreasing degreasing: add alkaline degreaser and carry out degreasing degreasing;
(3) acid pickling and rust removing: add acidic solution again and carry out acid pickling and rust removing;
(4) acid solution activation: the permanent magnet material after the pickling is activated in acid solution;
(5) plated film: the permanent magnet material after will activating is put into hair blackening liquid or the liquid that turns blue carries out plated film, forms black-and-blue or the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface.
According to the present invention, described hair blackening liquid comprises molybdate 13～60g/L; Aluminium salt 10～60g/L; Complexing agent 0～60g/L.Wherein, the consumption of described complexing agent is preferably 40～60g/L.
Wherein, described molybdate is ammonium molybdate or Sodium orthomolybdate; Described aluminium salt is aluminum chloride, Tai-Ace S 150, aluminum nitrate or aluminium ammonium sulfate; Described complexing agent comprises one or more components that are selected from ammoniacal liquor, EDTA, fluorochemical, oxalic acid, Trisodium Citrate, Tripotassium Citrate, Seignette salt and the SODIUM PHOSPHATE, MONOBASIC.Wherein, described fluorochemical is Sodium Fluoride, Potassium monofluoride or ammonium bifluoride.
According to the present invention, the described liquid that turns blue comprises alkali 110～190g/L, nitrite 60～170g/L, organic additive 10～60ml/L.Preferably, the described liquid that turns blue also comprises alkali 110～130g/L, nitrite 100～150g/L, organic additive 20～30ml/L.
Wherein, described alkali is sodium hydroxide or potassium hydroxide; Described nitrite is Sodium Nitrite or potassium nitrite; Described organic additive is ethylene glycol or glycerol.
According to the present invention, when using described hair blackening liquid to carry out plated film, temperature of reaction is 20～80 ℃, and the reaction times is 2～60 minutes, and preferably temperature of reaction is 40～60 ℃, and the reaction times is 5～60 minutes.When using the described liquid that turns blue to carry out plated film, temperature of reaction is 110～145 ℃, and the reaction times is 2～55 minutes, and preferably temperature of reaction is 110～120 ℃, and the reaction times is 10～15 minutes.
Wherein, in described degreasing degreasing, conventional sodium phosphate, yellow soda ash or the sodium hydroxide of using of described alkaline degreaser, their consumptions preferably are respectively 20～40g/L, 10～20g/L, 10～15g/L.
Wherein, in described acid pickling and rust removing, the conventional nitric acid that uses of described acidic solution, its consumption is preferably 1%～10%.
Wherein, in described acid solution activation, the conventional sulfuric acid that uses of described acid solution, its consumption is preferably 5%～10%.
According to the present invention, described black-and-blue protective membrane is a molybdenum aluminium protective membrane; Described mazarine protective membrane is that Z 250 is main, wherein also has the part rare earth oxide.
Advantage of the present invention and effect are:
The present invention utilizes the turn blue ultimate principle of the characteristics of black-emitting technology and Nd-Fe-Bo permanent magnet material and alumilite process of iron and steel to form a kind of chemoproection film on the neodymium iron boron surface.This chemoproection film can play the protective effect to Nd-Fe-B permanent magnet effectively, is adapted at using under the exsiccant condition.
The bonding force of black-and-blue protective membrane of the present invention and NdFeB material is good, protective membrane surface evenly, the solidity to corrosion height, the humid heat test (85 ℃ of temperature, humidity 80, relative humidity 100%) of PCT (high temperature and pressure test) and 3 hours has good preservative effect.
In addition, also be a very important problem as neodymium iron boron product high temperature loss of excitation.The high temperature demagnetize of black-and-blue protective membrane of the present invention also correspondingly is lower than like product (and the high temperature demagnetize of like product is 2～15%) between 0.1～1.6%.
One liter of solution of hair blackening liquid of the present invention can be handled 0.6 square metre Nd-Fe-Bo permanent magnet material.The hair blackening liquid good stability, solution was placed after one month, can also continue to produce.Do not contain the serious chemical ingredientss such as selenium of chemical pollution in the solution, environment-protecting asepsis is a kind of product of blackening agent for surface preferably.Can also realize the drum-type mass industrialized production in addition.
Embodiment
The present invention will be further described below with reference to embodiment, and embodiments of the invention only are 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 Nd-Fe-Bo permanent magnet material of ￠ 24*99*7mm were polished in vibrating ball mill 2 hours.Behind sodium phosphate 20g/L, yellow soda ash 10g/L, sodium hydroxide 10g/L degreasing degreasing, oxide on surface is removed in pickling in 1% nitric acid, washes 3 times, turns black after the activation of 5% sulfuric acid again.The Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into hair blackening liquid, hair blackening liquid consist of ammonium molybdate 13g/L, sulfate of ammoniac aluminium 40g/L.Under 45 ℃, reaction is 5 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 2 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 2
The Nd-Fe-Bo permanent magnet material of ￠ 24*9*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 2.5 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid.Hair blackening liquid consist of ammonium molybdate 13g/L, Tai-Ace S 150 40g/L, Sodium Fluoride 15g/L, EDTA 20g/L, ammoniacal liquor 10ml/L.Under 45 ℃, reaction is 5 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 2 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 3
The Nd-Fe-Bo permanent magnet material of ￠ 24*9*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 2.5 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid., hair blackening liquid consist of Sodium orthomolybdate 13g/L, Tai-Ace S 150 15g/L, Sodium Fluoride 5g/L.Under 40 ℃, reaction is 30 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 3 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 4
The Nd-Fe-Bo permanent magnet material of ￠ 24*9*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 2.5 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid.Hair blackening liquid consist of Sodium orthomolybdate 13g/L, Tai-Ace S 150 15g/L, EDTA30g/L, Seignette salt 10g/L.Under 20 ℃, reaction is 60 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 3 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 5
The Nd-Fe-Bo permanent magnet material of ￠ 10.4*6*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 3.5 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid.Hair blackening liquid consist of ammonium molybdate 13g/L, aluminium ammonium sulfate 15g/L, Trisodium Citrate 15g/L, oxalic acid 5g/L, Sodium Fluoride 5g/L.Under 45 ℃, reaction is 10 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 3 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 6
The Nd-Fe-Bo permanent magnet material of ￠ 24*99*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 2.3 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid.Hair blackening liquid consist of Sodium orthomolybdate 13g/L, Tai-Ace S 150 15g/L, Trisodium Citrate 15g/L, oxalic acid 10g/L, Sodium Fluoride 5g/L.Under 80 ℃, reaction is 2 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 3 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 7
The Nd-Fe-Bo permanent magnet material of ￠ 8*8*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 2.5 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid.Hair blackening liquid consist of ammonium molybdate 30g/L, aluminum chloride 13g/L, oxalic acid 50g/L, Sodium Fluoride 10g/L, under 50 ℃, reaction is 15 minutes in drum, forms black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out, wash 3 times, with the suds sealing, washing dries up packaging final prod again.
Embodiment 8
The Nd-Fe-Bo permanent magnet material of ￠ 8*8*7mm is pressed the polishing of embodiment 1 method, degreasing degreasing, acid-wash activation for 2.5 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into hair blackening liquid; hair blackening liquid consist of ammonium molybdate 60g/L, Tai-Ace S 150 60g/L, SODIUM PHOSPHATE, MONOBASIC 15g/L, Potassium monofluoride 15g/L, Seignette salt 15g/L; under 60 ℃; reaction formed black-and-blue protective membrane at neodymium-iron-boron permanent magnetic material surface after 20 minutes in drum.Nd-Fe-Bo permanent magnet material is taken out, wash 3 times, with the suds sealing, hot water wash dries up, packaging final prod.
Embodiment 9
With 5.0 kilograms of the Nd-Fe-Bo permanent magnet materials of ￠ 24.99*7mm, polishing 3 hours in vibrating ball mill earlier.Through sodium phosphate 30g/L, yellow soda ash 15g/L, behind the sodium hydroxide 15g/L degreasing degreasing, oxide on surface is removed in pickling in 5% nitric acid, washes 3 times, activates through 5% sulfuric acid again.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into the liquid that turns blue; this liquid that turns blue consists of the aqueous solution of sodium hydroxide 190g/L, Sodium Nitrite 170g/L, ethylene glycol 60ml/L; under 145 ℃, boiled 2 minutes, and formed the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out after washing 3 times, dry up packaging final prod.
Embodiment 10
The Nd-Fe-Bo permanent magnet material of ￠ 28*15*3mm is pressed the polishing of embodiment 9 methods, degreasing degreasing, pickling, activation for 4.6 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into the liquid that turns blue; this liquid that turns blue consists of the aqueous solution of potassium hydroxide 130g/L, potassium nitrite 150g/L, glycerine 30ml/L; under 120 ℃, boiled 10 minutes, and formed the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out after washing 3 times, dry up packaging final prod.
Embodiment 11
The Nd-Fe-Bo permanent magnet material of ￠ 28*15*3mm is pressed the polishing of embodiment 9 methods, degreasing degreasing, pickling, activation for 4.6 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into the liquid that turns blue; this liquid that turns blue consists of the aqueous solution of sodium hydroxide 110g/L, Sodium Nitrite 100g/L, ethylene glycol 20ml/L; under 110 ℃, boiled 15 minutes, and formed the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out after washing 2 times, dry up packaging final prod.
Embodiment 12
The Nd-Fe-Bo permanent magnet material of ￠ 28*15*3mm is pressed the polishing of embodiment 9 methods, degreasing degreasing, pickling, activation for 4.6 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into the liquid that turns blue, and this liquid that turns blue consists of the aqueous solution of sodium hydroxide 140g/L, Sodium Nitrite 80g/L, glycerine 45ml/L, boils under 130 ℃ 30 minutes, forms the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out after washing 2 times, dry up packaging final prod.
Embodiment 13
The Nd-Fe-Bo permanent magnet material of ￠ 28*15*3mm is pressed the polishing of embodiment 5 methods, degreasing degreasing, pickling, activation for 4.6 kilograms.The Nd-Fe-Bo permanent magnet material that pre-treatment is intact is put into the liquid that turns blue, and this liquid that turns blue consists of the aqueous solution of sodium hydroxide 110g/L, Sodium Nitrite 60g/L, glycerine 10ml/L, boils under 110 ℃ 55 minutes, forms the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface.Nd-Fe-Bo permanent magnet material is taken out after washing 2 times, dry up packaging final prod.
| Instance number | PCT (hour) | Damp and hot (hour) | High temperature demagnetize (%) |
| Example 1 | 3 | 3 | 1.3 |
| Example 2 | 4 | 3 | 0.7 |
| Example 3 | 3 | 3 | 1.4 |
| Example 4 | 3 | 3 | 1.2 |
| Example 5 | 5 | 4 | 0.1 |
| Example 6 | 5 | 3 | 0.3 |
| Example 7 | 3 | 3 | 1.6 |
| Example 8 | 3 | 3 | 1.2 |
| Example 9 | 6 | 6 | 1.0 |
| Example 10 | 6 | 6 | 0.5 |
| Example 11 | 4 | 4 | 1.1 |
| Example 12 | 6 | 6 | 0.3 |
| Example 13 | 6 | 6 | 0.1 |
Though introduce and described the specific embodiment of the present invention, the present invention is not limited thereto, but can also come specific implementation with the alternate manner in the scope that is in the technical scheme that defines in the claims.
Claims (9)
1, a kind of process for protecting surface of Nd-Fe-Bo permanent magnet material, described process for protecting surface comprises the steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that Nd-Fe-Bo permanent magnet material is polished;
(2) degreasing degreasing: add alkaline degreaser and carry out degreasing degreasing;
(3) acid pickling and rust removing: add acidic solution again and carry out acid pickling and rust removing;
(4) acid solution activation: the permanent magnet material after the pickling is activated in acid solution;
(5) plated film: the permanent magnet material after will activating is put into hair blackening liquid or the liquid that turns blue carries out plated film, forms black-and-blue or the mazarine protective membrane at neodymium-iron-boron permanent magnetic material surface;
Wherein, described hair blackening liquid comprises molybdate 13～60g/L, aluminium salt 10～60g/L, complexing agent 0～60g/L;
The described liquid that turns blue comprises alkali 110～190g/L, nitrite 60～170g/L, organic additive 10～60ml/L.
2, process for protecting surface according to claim 1 is characterized in that, the consumption of described complexing agent is 40～60g/L.
3, process for protecting surface according to claim 1 is characterized in that, the described liquid that turns blue also comprises alkali 110～130g/L, nitrite 100～150g/L, organic additive 20～30ml/L.
4, process for protecting surface according to claim 1 is characterized in that, described molybdate is ammonium molybdate or Sodium orthomolybdate; Described aluminium salt is aluminum chloride, Tai-Ace S 150, aluminum nitrate or aluminium ammonium sulfate; Described complexing agent comprises one or more components that are selected from ammoniacal liquor, EDTA, fluorochemical, oxalic acid, Trisodium Citrate, Tripotassium Citrate, Seignette salt and the SODIUM PHOSPHATE, MONOBASIC.
5, process for protecting surface according to claim 4 is characterized in that, described fluorochemical is Sodium Fluoride, Potassium monofluoride or ammonium bifluoride.
6, process for protecting surface according to claim 1 is characterized in that, described alkali is sodium hydroxide or potassium hydroxide; Described nitrite is Sodium Nitrite or potassium nitrite; Described organic additive is ethylene glycol or glycerol.
7, process for protecting surface according to claim 1 is characterized in that, when using described hair blackening liquid to carry out plated film, temperature of reaction is 20～80 ℃, and the reaction times is 2～60 minutes; When using the described liquid that turns blue to carry out plated film, temperature of reaction is 110～145 ℃, and the reaction times is 2～55 minutes.
According to claim 1 or 7 described process for protecting surface, it is characterized in that 8, when using described hair blackening liquid to carry out plated film, temperature of reaction is 40～60 ℃, the reaction times is 5～60 minutes; When using the described liquid that turns blue to carry out plated film, temperature of reaction is 110～120 ℃, and the reaction times is 10～15 minutes.
9, process for protecting surface according to claim 1 is characterized in that, described alkaline degreaser is sodium phosphate, yellow soda ash or sodium hydroxide; Described acidic solution is a nitric acid; Described acid solution is a sulfuric acid.
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| CNB2007100905969A CN100473759C (en) | 2007-04-12 | 2007-04-12 | Surface protection of neodymium iron boron permanent-magnet material |
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