CN100402698C - Electroless nickel-phosphorus plating process for Nd-Fe-Bo permanent magnet material - Google Patents

Electroless nickel-phosphorus plating process for Nd-Fe-Bo permanent magnet material Download PDF

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CN100402698C
CN100402698C CNB2006100381456A CN200610038145A CN100402698C CN 100402698 C CN100402698 C CN 100402698C CN B2006100381456 A CNB2006100381456 A CN B2006100381456A CN 200610038145 A CN200610038145 A CN 200610038145A CN 100402698 C CN100402698 C CN 100402698C
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plating
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acid
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CN1807682A (en
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鲁国强
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Abstract

The present invention discloses a chamical nickel-phosphorus plating method for Nd-Fe-Bo permanent magnetic materials. The method has the technical scheme that the chemical nickel-phosphorus plating method is carried out in the following way: hole sealing chemical plating is used for Nd-Fe-B hole sealing, and neutral chemical plating is used for thickening and blocking; acidic high-phosphorus chemical plating is carried out. The method comprises the steps of roll-finish chamfering, oil removal, rust removal, activation, hole-sealing chemical plating, neutral chemical plating, acidic high-phosphorus chemical plating, passivation, etc. The method has the characteristics of simple and easy realization of industrial application, low production cost and high performance-price ratios of products.

Description

A kind of chemical nickel and phosphor plating method of Nd-Fe-Bo permanent magnet material
Technical field
The present invention relates to the chemical conversion treatment field that the powder metallurgy material reaches corrosion susceptible materials in acid-base solution, specifically the chemical nickel and phosphor plating method of Nd-Fe-Bo permanent magnet material.
Background technology
Nd-Fe-B permanent magnet is the strongest permanent magnet material of present magnetic, has excellent properties and higher performance such as high energy product, high-coercive force, high remanent magnetism, and becomes the critical function material in the Modern High-Tech field.But because lanthanide series metal Nd is very active in damp atmosphere and acid-basicity solution, easily oxidized and corrosion, the powder metallurgy sintering process makes material surface have many micropores simultaneously, cause its surface to be difficult to handle and make its solidity to corrosion poor, the magnetic performance of permanent magnet is reduced greatly, have a strong impact on the application of permanent magnet.In the prior art, adopt technology such as organic coat method, plating and electroless plating for the surface treatment of NdFeB material more, obtained some effects, still have solidity to corrosion difference problem.Generally adopt chemical nickel plating coating in the world or electroplate the ambrose alloy nickel composite deposite as protective layer, wherein chemical nickel plating coating porosity is big, and anticorrosion effect is poor, has problems such as quality of coating instability in uneven thickness and contaminate environment and electroplate.Have report to adopt ultrasonic electroless deposition technique, neutral acid compound plating effect pretty good, but do not see industrial application, the ultrasonic electroless deposition technique industrial equipments is difficult to realize that neutral acid compound plating can't resolve the micropore problem of permanent magnet.
Summary of the invention
The objective of the invention is for the powder metallurgy material and in acid-base solution corrosion susceptible materials a kind of coating imporosity, the chemical nickel and phosphor plating method that thickness is even and solidity to corrosion is strong are provided.To achieve these goals, technical scheme of the present invention is to adopt the sealing of hole electroless plating to neodymium iron boron sealing of hole and neutral electroless plating thickening blocking-up, carries out the chemical nickel and phosphor plating method of acid high phosphorus chemical plating again.Comprise tumbling chamfering, oil removing, rust cleaning, activation, sealing of hole electroless plating, neutral electroless plating, acid high phosphorus chemical plating, passivation step, specific as follows:
1. tumbling chamfering
According to the NdFeB material of different size shape, corresponding employing vibration mill or drum-type shredder or centrifugal grinding mills are inserted NdFeB material and abrasive material and are carried out the tumbling chamfering in the shredder.
2. oil removing
Adopt the oil removing of ultrasonic wave alkali lye: under the ultrasonic wave state, carry out the alkali lye oil removing, alkali lye pH value is 8～10.5, and the alkali lye prescription is as follows:
Tertiary sodium phosphate Na 3PO 412H 2O:10～30g/l;
Yellow soda ash Na 2CO 3: 5～20g/l;
Emulsifier op-10: 1～5g/l;
Alkali liquid temperature is 50～80 ℃, adopts ultrasonic wave simultaneously, and ultrasonic frequency is that 20～80kHz, power are 50～500W, and the treatment time is 5～10 minutes;
3. rust cleaning
Adopt 1～3% HNO 3+ 0～1g/l thiocarbamide carries out pickling, and the time is 10～40 seconds; Temperature is a room temperature.
4. activation
Adopt citric acid 5～30g/l, Neutral ammonium fluoride 5～40g/l, temperature: room temperature, time: 5～20 seconds;
5. sealing of hole electroless plating
As reductive agent, single nickel salt adds complexing agent, low temperature accelerator as main salt to plating bath with inferior sodium phosphate, and the prescription of plating bath is as follows:
Single nickel salt NiSO 46H 2O:20～30g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:10～30g/l;
Sodium-acetate NaAC3H 2O:10～25g/l;
Glycine NH 2CH 2COOH:1～10g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:5～20g/l;
Neutral ammonium fluoride NH 4F 10～40g/l;
PH:6.5～8.5,50～70 ℃ of temperature, 1～15 minute time, plating speed is 10～30 μ m/ hours;
6. neutral electroless plating
Electroplate liquid formulation is as follows:
Single nickel salt NiSO 46H 2O:20～30g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:10～30g/l;
Sodium-acetate NaAC3H 2O:10～20g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:5～20g/l;
Lactic acid CH 3CHOCOOH:5～25ml/l;
Lead acetate: 1～5mg/l;
Thiocarbamide H 2NCSNH 2: 1～5mg/l;
Temperature: 60～80 ℃, pH:6.5～7.5,15～40 minutes time; 12～20 μ m/ hours;
7. acid high phosphorus chemical plating
Electroplate liquid formulation is as follows:
Single nickel salt NiSO 46H 2O:20～30g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:20～40g/l;
Sodium-acetate NaAC3H 2O:10～30g/l;
Lactic acid CH 3CHOCOOH:5～25ml/l;
DL-oxysuccinic acid CHOHCH 2(COOH) 2: 5～25g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:2～20g/l;
Succinic Acid (CH 2COOH) 2: 5～20g/l;
Lead acetate: 1～5mg/l;
Thiocarbamide H 2NCSNH 2: 1～5mg/l;
Temperature: 80～90 ℃, pH:4.4～4.8,40～60 minutes time; 12～16 μ m/ hours;
8. passivation
Adopt CrO 3Carry out Passivation Treatment, processing parameter:
CrO 3: 1～10g/l, temperature: 70～85 ℃, time: 10～20 minutes.
The chemical nickel and phosphor plating method of Nd-Fe-Bo permanent magnet material of the present invention utilizes three-dimensional chemical nickel phosphorus plating method layering time, even compact at matrix surface plating one deck from inside to outside, imporous nickel-phosphorus coating step by step.The preplating in the hole of neodymium iron boron of sealing of hole electroless plating elder generation plays the sealing of hole effect, neutral electroless plating is thickeied the effect of having blocked the sealing hole to hole and surface, make nickel-phosphorus coating matrix surface plating one deck even compact, low hole, matrix is played blocking effect, then, carry out the solidity to corrosion that acid high phosphorus chemical plating further improves coating again, play protective effect better matrix.
Beneficial effect of the present invention is as follows:
Coating imporosity thickness evenly and the matrix hole all by plating, thereby improved the corrosion resisting property of Nd-Fe-Bo permanent magnet material, avoided not caused coating bulge, skin effect phenomenon by plating because of the matrix hole.Sealing of hole electroless plating prescription, neutral electroless plating prescription, the acid high phosphorus chemical plating prescription of the application of the invention development adopt chemical nickel and phosphor plating method, play the protective effect to matrix better.
2. the present invention is when the nickel-phosphorus coating thickness of matrix surface formation reaches 25～30 microns, and damp and hot, High-Voltage Experimentation is more than 500 hours, and salt mist experiment is more than 200 hours.
The present invention realizes that industrial application is simple, and production cost is low, and product price ratio height can satisfy the demand for exports of domestic neodymium iron boron manufacturing enterprise, the problem in the reasonable solution actual production greatly.
Embodiment
Be described in further detail the present invention below by embodiment.
1. tumbling chamfering
Adopt vibration mill, NdFeB material and abrasive material are inserted carry out the tumbling chamfering in the shredder.
2. oil removing
Adopt the oil removing of ultrasonic wave alkali lye.Under the ultrasonic wave state, carry out the alkali lye oil removing, alkali lye pH value is 10.5, the alkali lye prescription is as follows:
Tertiary sodium phosphate Na 3PO 412H 2O:25g/l;
Yellow soda ash Na 2CO 3: 15g/l;
Emulsifier op-10: 1g/l;
Alkali liquid temperature is 50～80 ℃, adopts ultrasonic wave simultaneously, and ultrasonic frequency is that 40kHz, power are 500W, and the treatment time is 10 minutes;
3. rust cleaning
Adopt 2% HNO 3+ 0.25g/l thiocarbamide carries out pickling, and the time is 30 seconds; Temperature is a room temperature.
4. activation
Adopt citric acid 15g/l, Neutral ammonium fluoride 10g/l, temperature: room temperature, time: 15 seconds;
5. sealing of hole electroless plating
As reductive agent, single nickel salt adds complexing agent, low temperature accelerator as main salt to plating bath with inferior sodium phosphate, and the prescription of plating bath is as follows:
Single nickel salt NiSO 46H 2O:25g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:25g/l;
Sodium-acetate NaAC3H 2O:12g/l;
Glycine NH 2CH 2COOH:2g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:12g/l;
Neutral ammonium fluoride NH 4F 15g/l.
PH:7,65 ℃ of temperature, 10 minutes time, plating speed is 20 μ m/ hours;
6. neutral electroless plating electroplate liquid formulation is as follows:
Single nickel salt NiSO 46H 2O:25g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:20g/l;
Sodium-acetate NaAC3H 2O:10g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:12g/l;
Lactic acid CH 3CHOCOOH:25ml/l;
Lead acetate: 1mg/l,
Thiocarbamide H 2NCSNH 2: 1mg/l;
Temperature: 78 ℃, pH:6.5,30 minutes time; 15 μ m/ hours;
7. acid high phosphorus chemical plating
Single nickel salt NiSO 46H 2O:27g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:30g/l;
Sodium-acetate NaAC3H 2O:20g/l;
Lactic acid CH 3CHOCOOH:20ml/l;
DL-oxysuccinic acid CHOHCH 2(COOH) 2: 12g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:5g/l;
Succinic Acid (CH 2COOH) 2: 8g/l;
Lead acetate: 1mg/l,
Thiocarbamide H 2NCSNH 2: 1mg/l;
Temperature: 88 ℃, pH:4.4～4.8,90 minutes time; 15 μ m/ hours;
8. passivation
Adopt CrO 3Carry out Passivation Treatment, processing parameter:
CrO 3: 3g/l, temperature: 70 ℃, time: 10 minutes.
Relevant comparison sheet 1
Chemical plating method Salt mist experiment Damp and hot experiment The magnetic loss rate Outward appearance
Acidic bath 48 hours 172 hours 10～15％ Gloomy
Alkali plating solution 96 hours 720 hours 5～10％ Bright
Neutral plating bath 140 hours 960 hours 1～3％ Bright
The present invention 280 hours 1000 hours 1～3％ Light

Claims (1)

1. the chemical nickel and phosphor plating method of a Nd-Fe-Bo permanent magnet material, its method is: Nd-Fe-B permanent magnet is to be formed by the mmaterial sintering, surface irregularity has very high porosity and very easily corrosion in acid, basic solution; Adopt the sealing of hole electroless plating to neodymium iron boron sealing of hole and neutral electroless plating thickening blocking-up, carry out the chemical nickel and phosphor plating method of acid high phosphorus chemical plating again; Comprise tumbling chamfering, oil removing, rust cleaning, activation, sealing of hole electroless plating, neutral electroless plating, acid high phosphorus chemical plating, passivation step, technological process is as follows:
1) tumbling chamfering
According to the NdFeB material of different size shape, corresponding employing vibration mill or drum-type shredder or centrifugal grinding mills are inserted NdFeB material and abrasive material and are carried out the tumbling chamfering in the shredder;
2) oil removing
Adopt the oil removing of ultrasonic wave alkali lye: under the ultrasonic wave state, carry out the alkali lye oil removing, alkali lye pH value is 8～10.5, and the alkali lye prescription is as follows:
Tertiary sodium phosphate Na 3PO 412H 2O:10～30g/l;
Yellow soda ash Na 2CO 3: 5～20g/l;
Emulsifier op-10: 1～5g/l;
Alkali liquid temperature is 50～80 ℃, adopts ultrasonic wave simultaneously, and ultrasonic frequency is that 20～80kHz, power are 50～500W, and the treatment time is 5～10 minutes;
3) rust cleaning
Adopt 1～3% HNO 3+ 0～1g/l thiocarbamide carries out pickling, and the time is 10～40 seconds; Temperature is a room temperature;
4) activation
Adopt citric acid 5～30g/l, Neutral ammonium fluoride 5～40g/l, temperature: room temperature, time: 5～20 seconds;
5) sealing of hole electroless plating
As reductive agent, single nickel salt adds complexing agent, low temperature accelerator as main salt to plating bath with inferior sodium phosphate, and the prescription of plating bath is as follows:
Single nickel salt NiSO 46H 2O:20～30g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:10～30g/l;
Sodium-acetate NaAC3H 2O:10～25g/l;
Glycine NH 2CH 2COOH:1～10g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:5～20g/l;
Neutral ammonium fluoride NH 4F 10～40g/l;
PH:6.5～8.5,50～70 ℃ of temperature, 1～15 minute time, plating speed is 10～30 μ m/ hours;
6) neutral electroless plating
Electroplate liquid formulation is as follows:
Single nickel salt NiSO 46H 2O:20～30g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:10～30g/l;
Sodium-acetate NaAC3H 2O:10～20g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:5～20g/l;
Lactic acid CH 3CHOCOOH:5～25ml/l;
Lead acetate: 1～5mg/l;
Thiocarbamide H 2NCSNH 2: 1～5mg/l;
Temperature: 60～80 ℃, pH:6.5～7.5,15～40 minutes time; 12～20 μ m/ hours;
7) acid high phosphorus chemical plating
Electroplate liquid formulation is as follows:
Single nickel salt NiSO 46H 2O:20～30g/l;
Inferior sodium phosphate NaH 2PO 2H 2O:20～40g/l;
Sodium-acetate NaAC3H 2O:10～30g/l;
Lactic acid CH 3CHOCOOH:5～25ml/l;
DL-oxysuccinic acid CHOHCH 2(COOH) 2: 5～25g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:2～20g/l;
Succinic Acid (CH 2COOH) 2: 5～20g/l;
Lead acetate: 1～5mg/l;
Thiocarbamide H 2NCSNH 2: 1～5mg/l;
Temperature: 80～90 ℃, pH:4.4～4.8,40～60 minutes time; 12～16 μ m/ hours;
8) passivation
Adopt CrO 3Carry out Passivation Treatment, processing parameter:
CrO 3: 1～10g/l, temperature: 70～85 ℃, time: 10～20 minutes.
CNB2006100381456A 2006-01-26 2006-01-26 Electroless nickel-phosphorus plating process for Nd-Fe-Bo permanent magnet material Expired - Fee Related CN100402698C (en)

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CN100427642C (en) * 2006-05-11 2008-10-22 浙江大学 Method of raising binding force of chemical coating on the surface of NdFeB permanent magnet
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CN102189464A (en) * 2010-03-05 2011-09-21 肇庆三环京粤磁材有限责任公司 Method for chamfering inner bore on sintered neodymium-iron-boron magnet
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CN102560444B (en) * 2012-02-17 2013-12-11 湖南航天工业总公司 Process for chemically and compositely plating nickel, copper and phosphorus on sintered neodymium iron boron
CN102560445B (en) * 2012-02-17 2014-02-19 湖南航天工业总公司 Process for chemically and compositely plating nickel and phosphorus on sintered neodymium iron boron
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CN103060803B (en) * 2013-01-10 2014-12-03 西安科技大学 Method for preparing composite coating at surface of neodymium iron boron permanent magnet
CN103386412B (en) * 2013-07-09 2015-07-15 慈溪市共力磁业有限公司 Cleaning and recycling technology of neodymium iron boron waste
CN103451663B (en) * 2013-08-19 2015-09-02 南通保来利轴承有限公司 A kind of method of surface of rare earth permanent-magnetic process
CN103903851B (en) * 2014-04-04 2016-10-26 北京工业大学 A kind of method preparing corrosion-resistant Ne-Fe-B permanent magnet
CN105986255A (en) * 2015-02-16 2016-10-05 潘启荣 Surface treatment method of workpiece
CN106148955A (en) * 2015-03-26 2016-11-23 海安县建业磁材有限公司 A kind of surfacecti proteon processing method of samarium-cobalt permanent-magnetic material
CN105369226A (en) * 2015-12-07 2016-03-02 湖南航天磁电有限责任公司 Chemical nickel phosphor plating solution for surface acidity of sintered NdFeB magnet, and nickel phosphor plating process
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CN108221016B (en) * 2017-12-21 2019-10-01 广州传福化学技术有限公司 A kind of zinc-plated sealer and its application method
CN108411287A (en) * 2018-04-03 2018-08-17 沈阳工业大学 A kind of solution of low temperature acid Electroless Plating of Ni-P Alloy
CN109183099A (en) * 2018-10-30 2019-01-11 无锡鼎亚电子材料有限公司 It is a kind of for the weak caustic solution of oil removing to be electroplated
CN110453253A (en) * 2019-09-23 2019-11-15 合肥工业大学 A kind of preparation method of sintered NdFeB magnet surface NiP alloy layer
CN113005440A (en) * 2020-12-30 2021-06-22 昆明狴犴人力资源服务有限公司 Neodymium-iron-boron permanent magnet surface coating and preparation method thereof
CN113213524A (en) * 2021-06-01 2021-08-06 包头市华星稀土科技有限责任公司 Method for preparing praseodymium neodymium fluoride by using praseodymium neodymium oxalate

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