CN102115899A - Tin-nickel alloy plating solution used for plating neodymium iron boron permanent magnet material and method for plating neodymium iron boron permanent magnet material by adopting same - Google Patents
Tin-nickel alloy plating solution used for plating neodymium iron boron permanent magnet material and method for plating neodymium iron boron permanent magnet material by adopting same Download PDFInfo
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Abstract
The invention provides a tin-nickel alloy plating solution used for plating neodymium iron boron permanent magnet material and a method for plating neodymium iron boron permanent magnet material by adopting the same. The method for plating neodymium iron boron permanent magnet material comprises the following steps of: polishing the surface of the neodymium iron boron permanent magnet material through mechanical vibration grinding; degreasing and deoiling the polished neodymium iron boron permanent magnet material with a mixed degreasing fluid of sodium phosphate, sodium phosphate and sodium hydroxide; pickling and derusting the neodymium iron boron permanent magnet material with a salpeter solution; activating the pickled neodymium iron boron permanent magnet material with a sulfuric acid solution; and plating a tin-nickel alloy film on the activated neodymium iron boron permanent magnet material in a tin-nickel alloy plating solution. The method for plating neodymium iron boron permanent magnet material not only can reduce the thickness of the plated film, but also can greatly improve the corrosion resistance of the neodymium iron boron permanent magnet material.
Description
Technical field
The present invention relates to a kind of surface treatment method, particularly a kind of tin-nickel alloy plating bath that is used to electroplate Nd-Fe-Bo permanent magnet material, and adopt the tin-nickel alloy plating bath Nd-Fe-Bo permanent magnet material to be carried out the method for eleetrotinplate nickelalloy.
Background technology
Nd-Fe-Bo permanent magnet material is a kind of sintered magnetic material, and it forms a large amount of pores on the surface in the process of sinter molding, and these pores have increased follow-up galvanized difficulty.These pores can cause electroplating the back matrix and combine bad, electroplating solution with coating and can't be penetrated in the pore, and cause pore place coating to be put up a bridge, have a strong impact on the quality that neodymium-iron-boron permanent magnetic material surface is handled, and then influenced the corrosion resistance nature of Nd-Fe-Bo permanent magnet material.Nd-Fe-Bo permanent magnet material is as the magnetic king in the magneticsubstance, and its character is very active, is easy to be lost magnetism by the acid and alkali corrosion in the external world.So the quality that neodymium-iron-boron permanent magnetic material surface is handled is directly connected to the work-ing life and the performance of Nd-Fe-Bo permanent magnet material.
At present, the anti-corrosion method of Nd-Fe-Bo permanent magnet material has a lot.For example, publication number is that the Chinese invention patent application of CN1058053A discloses a kind of method of Nd-Fe-B alloys being carried out electronickelling, this method is for to carry out surface degreasing with the Nd-Fe-B alloys matrix with degreaser, after washing, immerse in the aqueous hydrochloric acid, after washing, put into basic solution again, after washing, be reentered in the aqueous hydrochloric acid again, put into plating bath after the washing again and electroplate.This application is having mentioned by its method that provides and can improve the corrosion resistance nature of Nd-Fe-B alloys general just, and any corrosion resistance nature data are not provided.
Publication number is that the Chinese invention patent application of CN 1448544A discloses a kind of neodymium-iron-boron permanent magnetic material surface guard technology, this technology adopts material surface electronickelling technology, in pre-treating technology, adopt the material surface hole sealing technology, in plating technology, adopt neutral plating bath plating compound coating technology of plating 1-3 hour in acidic bath immediately after 20-30 minute.Because this method needs to electroplate earlier neutral nickel, and then electroplates acid nickel, so complex process.
Chinese patent application CN 1058053A and CN 1448544A incorporate the present invention into as a reference at this.
And we know, Nd-Fe-Bo permanent magnet material for example is applied to all to have to face high temperature and moistening environment in air conditioner motor, electric motor of automobile or the elevator motor etc. usually, also may be applied to sometimes contain in the moisture of salinity.Therefore, require Nd-Fe-Bo permanent magnet material to have higher solidity to corrosion.
Summary of the invention
One object of the present invention has been to provide a kind of tin-nickel alloy plating bath that is used to electroplate Nd-Fe-Bo permanent magnet material, and described tin-nickel alloy plating bath comprises: tin protochloride 20～40 grams per liters, Nickel dichloride hexahydrate 20～40 grams per liters, potassium pyrophosphate 180～220 grams per liters, ammoniacal liquor 4～8ml/L, Padil 15～25 grams per liters, complexing agent 2～6 grams per liters.Wherein, described complexing agent is a quadrol.
Another purpose of the present invention has been to provide a kind of method of neodymium-iron boron permanent magnetic material electroplating tin-nickel alloy, said method comprising the steps of:
(1) chamfering polishing: adopt mechanical vibration that neodymium-iron-boron permanent magnetic material surface is polished;
(2) degreasing degreasing: use sodium phosphate, yellow soda ash and sodium hydroxide mixed defatting liquid that grinded Nd-Fe-Bo permanent magnet material is carried out degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that Nd-Fe-Bo permanent magnet material is carried out acid pickling and rust removing;
(4) acid solution activation: the Nd-Fe-Bo permanent magnet material after using sulphuric acid soln to pickling activates;
(5) zinc-plated nickelalloy film forming: in the tin-nickel alloy plating bath, the Nd-Fe-Bo permanent magnet material after the activation is carried out zinc-plated nickelalloy film forming, wherein, described tin-nickel alloy plating bath comprises: tin protochloride 20～40 grams per liters, Nickel dichloride hexahydrate 20～40 grams per liters, potassium pyrophosphate 180～220 grams per liters, ammoniacal liquor 4～8ml/L, Padil 15～25 grams per liters and complexing agent 2～6 grams per liters; Preferably, described complexing agent is a quadrol.
(6) aftertreatment: use the coating after hole sealing agent is handled plating.Preferably, described encapsulant is the agent of water-based nickel plating enclosure.The thickness of described coating is 12～18 microns.
Preferably, when electroplating, the temperature of described tin-nickel alloy plating bath is 45～55 ℃, and pH is 7.5～8.5, and current density is 0.5～1.5A/dm
2
Preferably, to use three road washed with de-ionized water coating before the sealing of hole.
Preferably, described Nd-Fe-Bo permanent magnet material is a sintered NdFeB
Preferably, using the hole sealing agent aftertreatment, the salt fog performance of coating is more than 240 hours.
According to method provided by the present invention, at first adopt the conventional mechanical vibration that neodymium-iron-boron permanent magnetic material surface is polished, help coating like this and combine better with matrix.With sodium phosphate, yellow soda ash and sodium hydroxide grinded Nd-Fe-Bo permanent magnet material is carried out conventional degreasing degreasing subsequently.In order to remove the oxide compound of neodymium-iron-boron permanent magnetic material surface, Nd-Fe-Bo permanent magnet material is carried out conventional acid pickling and rust removing with salpeter solution.In acid pickling and rust removing, the best lower nitric acid of working concentration, this is because the too high meeting of concentration of nitric acid causes pickling excessive, causes the magnetic property of Nd-Fe-Bo permanent magnet material to reduce; Concentration of nitric acid is too low then to cause pickling insufficient, has influence on the effect that erosion resistance is improved.
Behind the acid pickling and rust removing, water cleans Nd-Fe-Bo permanent magnet material, with sulphuric acid soln Nd-Fe-Bo permanent magnet material is carried out conventional activation treatment then, and this is pretreated final step, and the Nd-Fe-Bo permanent magnet material after activated can be electroplated.
The present invention uses the tin-nickel alloy plating bath that Nd-Fe-Bo permanent magnet material is electroplated, and uses tin instead of part nickel to reduce production costs.This tin-nickel alloy plating bath comprises tin protochloride 20～40 grams per liters, Nickel dichloride hexahydrate 20～40 grams per liters, potassium pyrophosphate 180～220 grams per liters, ammoniacal liquor 4～8ml/L, Padil 15～25 grams per liters and complexing agent 2～6 grams per liters, wherein add complexing agent and help the stable of plating bath, improve all platings and the covering power of plating bath, improve the coating outward appearance simultaneously.
Method provided by the invention can also comprise post-processing step, promptly the Nd-Fe-Bo permanent magnet material after electroplating is carried out sealing of hole and handles.Carrying out using deionized water that tin-nickel alloy coating is cleaned earlier before sealing of hole handles, such cleaning is carried out three times at least, has only tin-nickel alloy coating cleaned to guarantee the sealing of hole effect.Handle the porosity that can further reduce coating through sealing of hole, improved the salt fog performance of Nd-Fe-Bo permanent magnet material.
The method of neodymium-iron boron permanent magnetic material electroplating tin-nickel alloy provided by the present invention has the following advantages:
(1) compare for the method that the Chinese invention patent application of CN 1448544A is provided with publication number, this method only needs reduce operation sequence to neodymium-iron boron permanent magnetic material electroplating one deck tin-nickel alloy, enhances productivity.
(2) use the tin-nickel alloy plating bath that Nd-Fe-Bo permanent magnet material is electroplated, on the Nd-Fe-Bo permanent magnet material matrix, form tin-nickel alloy coating, that is to say and use tin to replace a part of nickel, so not only combine the advantage of tin, these two kinds of metals of nickel, and saved expensive nickel metal, reduced production cost.
(3) use method provided by the invention, can not only reduce the thickness of coating, and can improve the corrosion resistance nature of Nd-Fe-Bo permanent magnet material.Usually, the coating of Nd-Fe-Bo permanent magnet material is thick more, and its corrosion resistance nature is good more, but employed metal is also just many more, has increased cost widely.Compare with traditional nickel plating method, method provided by the invention is by using specific tin-nickel alloy plating bath, and the temperature and the pH of current density in the control electroplating process and tin-nickel alloy plating bath, in thickness of coating only is under 60～70% the situation of traditional nickel plating thickness of coating, has increased substantially the corrosion resistance nature of Nd-Fe-Bo permanent magnet material.For example, in document " neodymium iron boron magnetic body protection against corrosion research " (2000 " magnetics and magneticsubstance collected works " magnetics and magneticsubstance collected works (two) P89) disclosed method, thickness of coating reaches more than 20 microns, but the salt fog performance of Nd-Fe-Bo permanent magnet material is no more than 100 hours; And use method provided by the invention, thickness of coating only to be 12～18 microns, the salt fog performance of Nd-Fe-Bo permanent magnet material reached more than 240 hours.
(4) method provided by the invention has further reduced the porosity of coating by effective sealing of hole aftertreatment, has improved the salt fog performance of Nd-Fe-Bo permanent magnet material.
(5) method provided by the invention is a kind of electroplating technology of alkaline non-cyanide, employed plating bath environment-protecting asepsis, and plating bath is little to environment and equipment corrosion, and wastewater treatment is convenient.
The method that the application of the invention provided, can significantly improve the solidity to corrosion of Nd-Fe-Bo permanent magnet material, can make prepared Nd-Fe-Bo permanent magnet material have use range widely like this, can be applied to high temperature such as air conditioner motor, electric motor of automobile or elevator motor, moistening environment.Simultaneously, also make prepared Nd-Fe-Bo permanent magnet material have longer work-ing life.
Embodiment
For making your auditor can further understand structure of the present invention, feature and other purposes, 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.
In the present invention, employed Nd-Fe-Bo permanent magnet material can prepare by any method known to those skilled in the art.For example, prepare alloy pig by certain alloy formula melting, and this alloy pig is carried out broken powder process, and obtain pressed compact, subsequently pressed compact is carried out sintering in vacuum sintering furnace, carry out temper at last and obtain the agglomerating Nd-Fe-Bo permanent magnet material by moulding.
Embodiment 1
The sintered Nd-Fe-B permanent magnetic material of 3 kilograms of D15*4 was polished in vibrating ball mill 3 hours.Use the grease-removing agent of 10L, it consists of sodium phosphate 30g/ liter, yellow soda ash 8g/ rises and sodium hydroxide 8g/ liter, after Nd-Fe-Bo permanent magnet material carried out degreasing degreasing, remove the oxide compound of neodymium-iron-boron permanent magnetic material surface with 5% salpeter solution pickling, water cleans 3 times then.With 5% sulphuric acid soln Nd-Fe-Bo permanent magnet material is activated again, electroplate subsequently, the Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into the tin-nickel alloy plating bath, consisting of of this tin-nickel alloy plating bath: tin protochloride 20 grams per liters, Nickel dichloride hexahydrate 20 grams per liters, potassium pyrophosphate 180 grams per liters, ammoniacal liquor 4ml/L, Padil 15 grams per liters, complexing agent quadrol are 2 grams per liters.When electroplating, the temperature of tin-nickel alloy plating bath is that 45 ℃, pH are 7.5, and current density is 0.5A/dm
2, electroplating time is 200min.After electroplating end, the thickness of tin-nickel alloy coating is 18 microns.With washed with de-ionized water tin-nickel alloy coating three times, Nd-Fe-Bo permanent magnet material is crossed hole sealing agent and is carried out sealing of hole then, dries up the moisture of neodymium-iron-boron permanent magnetic material surface behind the sealing of hole with blower, dries 20min at last in 100 ℃ baking oven.Wherein, employed hole sealing agent is the NF1080 water-based nickel plating enclosure agent of being produced by Guangzhou Tianzhi Environmental Protection Science and Technology Co., Ltd..
Embodiment 2
The sintered Nd-Fe-B permanent magnetic material of 3 kilograms of D15*4 was polished in vibrating ball mill 3 hours.Use the grease-removing agent of 10L, it consists of sodium phosphate 30g/ liter, yellow soda ash 8g/ rises and sodium hydroxide 8g/ liter, after Nd-Fe-Bo permanent magnet material carried out degreasing degreasing, remove the oxide compound of neodymium-iron-boron permanent magnetic material surface with 5% salpeter solution pickling, water cleans 3 times then.With 5% sulphuric acid soln Nd-Fe-Bo permanent magnet material is activated again, electroplate subsequently, the Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into the tin-nickel alloy plating bath, the consisting of of this tin-nickel alloy plating bath: tin protochloride 30 grams per liters, Nickel dichloride hexahydrate 30 grams per liters, potassium pyrophosphate 200 grams per liters, ammoniacal liquor 6ml/L, Padil 20 grams per liters, complexing agent quadrol 4 grams per liters.When electroplating, the temperature of tin-nickel alloy plating bath is that 50 ℃, pH are 8.0, and current density is 1A/dm
2, electroplating time is 100min.After electroplating end, the thickness of tin-nickel alloy coating is 15 microns.With washed with de-ionized water tin-nickel alloy coating three times, Nd-Fe-Bo permanent magnet material is crossed pore-sealing liquid and is carried out sealing of hole then, dries up the moisture of neodymium-iron-boron permanent magnetic material surface behind the sealing of hole with blower, dries 20min at last in 100 ℃ baking oven.Wherein, employed hole sealing agent is the NF1080 water-based nickel plating enclosure agent of being produced by Guangzhou Tianzhi Environmental Protection Science and Technology Co., Ltd..
Embodiment 3
The sintered Nd-Fe-B permanent magnetic material of 3 kilograms of D15*4 was polished in vibrating ball mill 3 hours.Use the grease-removing agent of 10L, it consists of sodium phosphate 30g/ liter, yellow soda ash 8g/ rises and sodium hydroxide 8g/ liter, after Nd-Fe-Bo permanent magnet material carried out degreasing degreasing, remove the oxide compound of neodymium-iron-boron permanent magnetic material surface with 5% salpeter solution pickling, water cleans 3 times then.With 5% sulphuric acid soln Nd-Fe-Bo permanent magnet material is activated again, electroplate subsequently, the Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into the tin-nickel alloy plating bath, consisting of of this tin-nickel alloy plating bath: tin protochloride 40 grams per liters, Nickel dichloride hexahydrate 40 grams per liters, potassium pyrophosphate 220 grams per liters, ammoniacal liquor 8ml/L, Padil 25 grams per liters, when complexing agent quadrol 6 grams per liters are electroplated, the temperature of tin-nickel alloy plating bath is that 55 ℃, pH are 8.5, and current density is 1.5A/dm
2, electroplating time is 60min.After electroplating end, the thickness of tin-nickel alloy coating is 12 microns.With washed with de-ionized water tin-nickel alloy coating three times, Nd-Fe-Bo permanent magnet material is crossed pore-sealing liquid and is carried out sealing of hole then, dries up the moisture of neodymium-iron-boron permanent magnetic material surface behind the sealing of hole with blower, dries 20min at last in 100 ℃ baking oven.Wherein, employed hole sealing agent is the NF1080 water-based nickel plating enclosure agent of being produced by Guangzhou Tianzhi Environmental Protection Science and Technology Co., Ltd..
The comparative example 1
The sintered Nd-Fe-B permanent magnetic material of 3 kilograms of D15*4 was polished in vibrating ball mill 3 hours.Use the grease-removing agent of 10L, it consists of sodium phosphate 30g/ liter, yellow soda ash 8g/ rises and sodium hydroxide 8g/ liter, after Nd-Fe-Bo permanent magnet material carried out degreasing degreasing, remove the oxide compound of neodymium-iron-boron permanent magnetic material surface with 5% salpeter solution pickling, water cleans 3 times then.With 5% sulphuric acid soln Nd-Fe-Bo permanent magnet material is activated again, electroplate subsequently, the Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into a watt nickel solution, consisting of of this watt nickel plating bath: single nickel salts 200 grams per liters, Nickel dichloride hexahydrate 40 grams per liters, boric acid 50 grams per liters, wetting agent sodium lauryl sulphate 0.2 grams per liter, the temperature of plating bath is that 50 ℃, pH value are 4.0, and current density is 1.0A/dm
2, electroplating time is 100min.The thickness of coating is 25 microns.With deionized water cleaning workpiece three times, Nd-Fe-Bo permanent magnet material is crossed pore-sealing liquid and is carried out sealing of hole then, dries up the moisture of neodymium-iron-boron permanent magnetic material surface behind the sealing of hole with blower, dries 20min at last in 100 ℃ baking oven.Wherein, employed hole sealing agent is the NF1080 water-based nickel plating enclosure agent of being produced by Guangzhou Tianzhi Environmental Protection Science and Technology Co., Ltd..
The file experiment
Each 100 of Nd-Fe-Bo permanent magnet materials getting the prepared electronickelling of the Nd-Fe-Bo permanent magnet material of the prepared eleetrotinplate nickelalloy of embodiment 1-3 and comparative example 1 carry out the file experiment.Experimental technique is as follows: after the Nd-Fe-Bo permanent magnet material sample was decided with platform tiger clamping, with the edge of file filing sample, file face and sample coating surface were 45 °, file to the coating direction from matrix metal.Behind the repetition aforesaid operations 5 times, observe the position of filing, the coating of specimen surface is qualified not leave matrix metal, otherwise is defective, and the file experimental result is listed in the table 1.
Table 1
| Example | Experiment quantity | Qualified quantity |
| Example 1 | 100 | 100 |
| Example 2 | 100 | 100 |
| Example 3 | 100 | 100 |
| Comparison example 1 | 100 | 80 |
High temperature and pressure test and salt-fog test
Each 100 of Nd-Fe-Bo permanent magnet materials getting the prepared electronickelling of the Nd-Fe-Bo permanent magnet material of the prepared eleetrotinplate nickelalloy of embodiment 1-3 and comparative example 1 carry out high temperature and pressure test.The condition of high temperature and pressure test is: 120 ℃ of 2 normal atmosphere of container pressure, vessel temps, humidity is 100%.The High Temperature High Pressure senile experiment case that experimental installation is produced for great Yu's instrument Science and Technology Co., Ltd., model is PCT-35.The judging criterion of high temperature and pressure test is: coating does not have cracking, peeling, the no red rust in surface.The results are shown in Table 2 for high temperature and pressure test.
Each 100 of Nd-Fe-Bo permanent magnet materials getting the prepared electronickelling of the Nd-Fe-Bo permanent magnet material of the prepared eleetrotinplate nickelalloy of embodiment 1-3 and comparative example 1 carry out salt-fog test.The condition of salt-fog test is: brine concentration 5%, salt fog the temperature inside the box are 35 ℃, and the pressure pot temperature is 47 ℃, and spray pattern is spraying continuously.Experimental installation is the accurate salt spray testing machine that Qingdao Sol experimental installation company limited produces.The judging criterion of salt-fog test is: coating surface does not have red rust.The results are shown in Table 2 for salt-fog test.
Table 2 has shown the eleetrotinplate nickelalloy of embodiment 1-3 and comparative example's 1 the high temperature and pressure test of Nd-Fe-Bo permanent magnet material of electronickelling and the result of salt-fog test:
Table 2
| Example | High temperature and pressure test/hour | Salt-fog test/hour |
| Embodiment 1 | ＞96 | ＞240 |
| Embodiment 2 | ＞96 | ＞240 |
| Embodiment 3 | ＞96 | ≥240 |
| Embodiment 4 | ≤72 | ≤100 |
What need statement is 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 the qualification to 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. tin-nickel alloy plating bath that is used to electroplate Nd-Fe-Bo permanent magnet material, it is characterized in that described tin-nickel alloy plating bath comprises: tin protochloride 20～40 grams per liters, Nickel dichloride hexahydrate 20～40 grams per liters, potassium pyrophosphate 180～220 grams per liters, ammoniacal liquor 4～8ml/L, Padil 15～25 grams per liters, complexing agent 2～6 grams per liters.
2. tin-nickel alloy plating bath according to claim 1 is characterized in that, described complexing agent is a quadrol.
3. the method for a neodymium-iron boron permanent magnetic material electroplating tin-nickel alloy is characterized in that, said method comprising the steps of:
(1) chamfering polishing: adopt mechanical vibration that neodymium-iron-boron permanent magnetic material surface is polished;
(2) degreasing degreasing: use sodium phosphate, yellow soda ash and sodium hydroxide mixed defatting liquid that grinded Nd-Fe-Bo permanent magnet material is carried out degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that Nd-Fe-Bo permanent magnet material is carried out acid pickling and rust removing;
(4) acid solution activation: the Nd-Fe-Bo permanent magnet material after using sulphuric acid soln to pickling activates;
(5) zinc-plated nickelalloy film forming: in the tin-nickel alloy plating bath, the Nd-Fe-Bo permanent magnet material after the activation is carried out zinc-plated nickelalloy film forming, wherein, described tin-nickel alloy plating bath comprises: tin protochloride 20～40 grams per liters, Nickel dichloride hexahydrate 20～40 grams per liters, potassium pyrophosphate 180～220 grams per liters, ammoniacal liquor 4～8ml/L, Padil 15～25 grams per liters and complexing agent 2～6 grams per liters;
(6) aftertreatment: use the coating after hole sealing agent is handled plating.
4. method according to claim 3 is characterized in that, when electroplating, the temperature of described tin-nickel alloy plating bath is 45～55 ℃, and pH is 7.5～8.5, and current density is 0.5～1.5A/dm
2
5. method according to claim 3 is characterized in that, described complexing agent is a quadrol.
6. method according to claim 3 is characterized in that, described encapsulant is the agent of water-based nickel plating enclosure.
7. method according to claim 3 is characterized in that, the thickness of described coating is 12～18 microns.
8. method according to claim 3 is characterized in that, will use three road washed with de-ionized water coating before the sealing of hole.
9. according to each described method of claim 3～8, it is characterized in that described Nd-Fe-Bo permanent magnet material is a sintered NdFeB.
10. according to each described method of claim 3～8, it is characterized in that using the hole sealing agent aftertreatment, the salt fog performance of coating is more than 240 hours.
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