CN100498987C - Method for bonderizing sintered neodymium ferroboron magnetic material - Google Patents
Method for bonderizing sintered neodymium ferroboron magnetic material Download PDFInfo
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- CN100498987C CN100498987C CNB200610172643XA CN200610172643A CN100498987C CN 100498987 C CN100498987 C CN 100498987C CN B200610172643X A CNB200610172643X A CN B200610172643XA CN 200610172643 A CN200610172643 A CN 200610172643A CN 100498987 C CN100498987 C CN 100498987C
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Abstract
This invention discloses a phosphorization method for sintering NdFeB magnetic matrials, which applies a physical hole-sealing method to seal holes of a sintered NdFeB magnetic material and then carries out phosphorization and passivation including: cleaning chamfers-sealing holes-removing oil-removing rust-adjusting the surface-phosphorizing under normal temperature-passivation, which is suitable for industrial production and has strong ability of anticorrosion.
Description
The present invention relates to the surperficial organic coat pre-treatment field of sintered Nd-Fe-B magnetic material. specifically be exactly the phosphatization of sintered Nd-Fe-B magnetic material.
Nd-Fe-Bo permanent magnet material is widely used in high-new industries such as computer, telecommunications, information system, micromachine, automobile, nulcear magnetic resonance (NMR), instrument and meter because of it has high saturation and magnetic intensity, coercive force and big magnetic energy product.Nd-Fe-Bo permanent magnet material is the product by powder metallurgy sintered moulding, and short texture, porosity height, surface state are not good.The neodymium standard electrode potential is also more negative than iron, very easily oxidized in malaria, and corrode with airborne acidic materials generation kickback, intercrystalline corrosion very easily produced, form the oxide and the hydride of neodymium and cause the material efflorescence, thereby reduce and destroy the magnetic property of material.The defective of the caused corrosion-resistant of Nd-Fe-Bo permanent magnet material architectural characteristic has had a strong impact on its application in high-end magnetic product.The protective coating method is to improve one of the NdFeB material corrosion resistance very important approach, and phosphating process has been widely used in the industrial production as a kind of important surface treatment method, and it can significantly improve the adhesion and the decay resistance of coating and matrix.The organic coat of Nd-Fe-Bo permanent magnet material employing at present, its pre-treatment deoiling effect is undesirable, the phosphating process at medium temperature poor stability, the energy consumption height, the phosphating coat corrosion resistance that forms is low, matrix is with to be coated with binding force of membrane low, and the phosphatization of Nd-Fe-Bo permanent magnet material is to influence its organic coat technology key in application.
Purpose of the present invention in order to overcome and to solve the problem that prior art exists, on the basis of iron and steel normal-temperature zinc series and normal temperature iron system, provides a cover complete just, is fit to industrial Coating Pretreatment technology.To satisfy the surperficial organic coat requirement of domestic and international sintered Nd-Fe-B magnetic material.
The object of the present invention is achieved like this:
1, the method for bonderizing of sintered Nd-Fe-B magnetic material, its technology comprises: the tumbling chamfering, and---------------normal temperature phosphating---steps such as passivation are adjusted on the surface to sealing of hole in rust cleaning in oil removing.It is characterized in that:
A), tumbling chamfering
Adopt oscillating mill, drum-type grinder, centrifugal grinding mills, the sintered Nd-Fe-B magnetic material of different size and abrasive material are inserted grinder carry out grinder.
B), sealing of hole
2, sintered Nd-Fe-B magnetic material rough surface has very high porosity, and very easily corrosion in acidity, alkaline solution adopts method of pore sealing to its sealing of hole, can improve its corrosion stability.Its method is: the sintered Nd-Fe-B magnetic material of tumbling chamfering is put into the zinc stearate molten mass, and temperature is 150～160 ℃, 10 minutes time.Take out, cool off, remove the zinc stearate that solidifies, sealing of hole finishes.
C), oil removing
The sintered Nd-Fe-B magnetic material of tumbling chamfering, sealing of hole is put into degreasing fluid, and degreaser can be the neutral surface active agent; Neutral surface active agent and anion surfactant compound; Anion surface active and inorganic alkaline compound compound.Temperature is a normal temperature to 70 ℃.Also can strengthen with ultrasonic wave.Time eliminates to the neodymium-iron-boron magnetic material greasy dirt, and the surface is evenly wetting.
D), rust cleaning
Adopt 1～3%HNO
3+ 0～1% corrosion inhibiter, 10～40 seconds time, normal temperature.
E), the surface is adjusted
Adopt 0.05～0.1% glue titanium to make surface conditioner, 60～90 seconds time, normal temperature.
F), normal temperature phosphating
Adopt the normal-temperature zinc series phosphatization: total acid 25～30 points; Total acid 1.2～1.5 points; Total acid/total acid=20:1; Promoter 1 point; PH=2.8～3.2: normal temperature 10～15 minutes makes surface of the work form phosphating coat.
Adopting normal temperature iron is phosphatization: do not carry out surface adjustment before the phosphatization, do not add promoter.Total acid 12～16 points; PH=2.1～2.8; Normal temperature 10～15 minutes makes surface of the work form phosphating coat.
G), passivation
After phosphating coat forms, adopt Cr
6+Solution is done the passivator passivation, 1～3 minute time.
H), washing
After the phosphating coat passivation, carry out running water washing, distilled water washing, oven dry.
Be described in further detail the present invention below by embodiment.
1, tumbling chamfering
Adopt oscillating mill, drum-type grinder, centrifugal grinding mills, the sintered Nd-Fe-B magnetic material of different size and abrasive material are inserted grinder carry out grinder.
2, sealing of hole
The sintered Nd-Fe-B magnetic material rough surface has very high porosity, and very easily corrosion in acidity, alkaline solution adopts method of pore sealing to its sealing of hole, can improve its corrosion stability.Its method is: the sintered Nd-Fe-B magnetic material of tumbling chamfering is put into the zinc stearate molten mass, after a period of time, take out, cool off, remove the zinc stearate that solidifies, sealing of hole finishes.
3, oil removing
The sintered Nd-Fe-B magnetic material of tumbling chamfering, sealing of hole is put into degreasing fluid, and degreaser is 1%OP--10 neutral surface active agent and 1% neopelex anion surfactant compound, and surplus is formed by water.Normal temperature, the time eliminates to the neodymium-iron-boron magnetic material greasy dirt, and the surface is evenly wetting.
Perhaps use and consist of OP-10 emulsifying agent 2.5ml/l sodium carbonate 25g/l; Tertiary sodium phosphate 15g/l; Sodium phosphate trimer 5g/l; Surplus is the degreaser of water, and PH is less than 10; 50～70 ℃ of temperature.Eliminate to the neodymium-iron-boron magnetic material greasy dirt, the surface is evenly wetting.
Surface of the work behind the sealing of hole has adhered to a lot of hole sealing agents and must remove, and adopts the method for ultrasonic waves for cleaning, utilizes its " cavitation " effect to remove remaining hole sealing agent and has better effect, and can strengthen oil removing.
3, rust cleaning
Derusting process is for adopting 3%HNO
3+ 1% urea, 10～40 seconds time, normal temperature.Careful evenly to surface of the work, silvery white metallic luster is arranged
6, the surface is adjusted
Adopt 0.05～0.1% glue titanium to make surface conditioner, 60～90 seconds time, normal temperature.
7, adopt the normal-temperature zinc series phosphatization: total acid 25～30 points: total acid 1.2～1.5 points; Total acid/total acid=20:1; Promoter 1 point: PH=2.8～32; Normal temperature 10～15 minutes makes surface of the work form phosphating coat.
Adopting normal temperature iron is phosphatization: do not carry out surface adjustment before the phosphatization, do not add promoter.Total acid 12～16 points; PH=2.1～2.8; Normal temperature 10～15 minutes makes surface of the work form phosphating coat.
The normal-temperature zinc series phosphatization is the KH501 normal-temperature zinc series phosphatization liquid that this employing company produces, and KH501 normal-temperature zinc series phosphatization liquid is made up of nickel salt, phosphoric acid, zinc dihydrogen phosphate, zinc nitrate, molybdate, fluoride, organic acid complex compound.
Normal temperature iron is that phosphatization is the KH606 normal temperature phosphating liquor of iron series that this employing company produces, normal temperature phosphating liquor of iron series: do not carry out surface adjustment before the phosphatization, do not add promoter.The KH606 phosphating liquor of iron series is made up of nickel salt, phosphoric acid, sodium dihydrogen phosphate, molybdate, fluoride, organic acid complex compound.
8, passivation
The workpiece that phosphatization is good is put into the passivating solution passivation, and passivating solution is: chromic anhydride 3g/l, temperature 60～70; 2 minutes.
9, washing
After the phosphating coat passivation, carry out running water washing, distilled water washing, oven dry.
The phosphating coat corrosion resistance is measured
Measure corrosion resistance with cupric sulphate dropping test.Solution composition is: 0.2mol/LCuSO
45H
2O 40mL; 10%NaCl 20mL; 0.1mol/LHCl 0.8mL.Above-mentioned mixed liquor is dropped on the phosphating coat,
The rete porosity measurement
With reference to GB/T17721-1999 " test of metal cladding ferroxyl test ferron ", measure the porosity of phosphorization membrane, solution composition is: potassium ferricyanide 10g/L, sodium chloride 20g/L, the filter paper stickup time is 10min, will be printed on the filter paper of spot then, behind distilled water flushing, be placed on the clean glass plate, porosity is calculated according to blob features in dry back, with individual/cm
2Expression.
Salt mist test
Standard GB/T 10125-1997 with reference to neutral salt spray test carries out salt mist test, observes the specimen surface corrosion condition.
The phosphating coat performance
| Corrosion resistance (s) porosity is (individual/cm 2) salt mist test (hour) |
| Zinc phosphating 0 12 2 iron be behind phosphatization 0 12 1 sealing of holes behind Zinc phosphating 30 0.5 8 sealing of holes iron be phosphatization 20 0.5 8 |
Find out that from last table the sintered Nd-Fe-B magnetic material phosphatization of carrying out according to the present invention GB6807-86 steel surface pre-treatment requirement that has been up to state standards has practicality, can satisfy sintered Nd-Fe-B magnetic material and be coated with reload request.
Claims (3)
1, a kind of method for bonderizing of sintered Nd-Fe-B magnetic material, its technology comprises: the tumbling chamfering---sealing of hole---oil removing---rust cleaning---normal temperature phosphating---passivation---water-washing step is characterized in that:
A), tumbling chamfering
Adopt oscillating mill, drum-type grinder, centrifugal grinding mills, the sintered Nd-Fe-B magnetic material of different size and abrasive material are inserted grinder grind;
B), sealing of hole
The sintered Nd-Fe-B magnetic material rough surface, has very high porosity, very easily corrosion in acidity, alkaline solution, adopt method of pore sealing to its sealing of hole, can improve its corrosion stability, its method is: the sintered Nd-Fe-B magnetic material of tumbling chamfering is put into the zinc stearate molten mass, after-section the time, take out, cool off, remove the zinc stearate that solidifies, sealing of hole finishes;
C), oil removing
The sintered Nd-Fe-B magnetic material of tumbling chamfering, sealing of hole is put into degreaser, and degreaser is 1%OP-10 neutral surface active agent and 1% neopelex anion surfactant compound, and surplus is formed by water, normal temperature; Perhaps degreaser is OP-10 emulsifying agent 2.5ml/1, sodium carbonate 25g/l, tertiary sodium phosphate 15g/l, sodium phosphate trimer 5g/l, surplus is formed by water, and pH is less than 10,50～70 ℃ of temperature, strengthen with ultrasonic wave, the time eliminates to the sintered Nd-Fe-B magnetic material greasy dirt, and the surface is evenly wetting;
D), rust cleaning
Adopt 3%HNO
3+ 1% urea, 10～40 seconds time, normal temperature;
E), normal temperature phosphating
Adopting normal temperature iron is phosphatization: do not carry out surface adjustment before the phosphatization, do not add promoter, and total acid 12～16 points, pH=2.1～2.8, normal temperature 10～15 minutes makes surface of the work form phosphating coat; Phosphating liquor of iron series is made up of nickel salt, phosphoric acid, sodium dihydrogen phosphate, molybdate, fluoride, organic acid complex compound;
G), passivation
After phosphating coat forms, adopt Cr
6+Solution is done the passivator passivation, 1～3 minute time;
H), washing
After the phosphating coat passivation, carry out running water washing, distilled water washing, oven dry.
2, method according to claim 1 is characterized in that described sealing of hole is 150～160 ℃ with the zinc stearate melt temperature, 10 minutes time.
3, method according to claim 1 is characterized in that described passivator is chromic anhydride 3g/l, temperature 60～70; 2 minutes.
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| CNB200610172643XA CN100498987C (en) | 2006-10-28 | 2006-12-28 | Method for bonderizing sintered neodymium ferroboron magnetic material |
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| CN200610143408 | 2006-10-28 | ||
| CNB200610172643XA CN100498987C (en) | 2006-10-28 | 2006-12-28 | Method for bonderizing sintered neodymium ferroboron magnetic material |
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| CN100498987C true CN100498987C (en) | 2009-06-10 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102605361B (en) * | 2011-01-24 | 2016-11-23 | 北京中科三环高技术股份有限公司 | A kind of surface treatment method of sintered Nd-Fe-B magnetic material |
| CN102424963B (en) * | 2011-12-23 | 2013-09-18 | 无锡鸿海龙船机有限公司 | Phosphate treatment technology for deformation-free scuffing-resistant inner sleeve |
| CN103805983B (en) * | 2012-11-08 | 2018-08-21 | 北京中科三环高技术股份有限公司 | A kind of permanent-magnet material carries out parkerized surface treatment method using bonderite |
| CN103498139B (en) * | 2013-09-24 | 2015-09-30 | 宁波韵升粘结磁体有限公司 | A kind of method improving neodymium iron boron magnetic body antiseptic property |
| CN104637664B (en) * | 2013-11-14 | 2018-08-07 | 天津三环乐喜新材料有限公司 | A kind of preparation method of corrosion resistance Nd-Fe-B permanent magnet |
| CN103996525A (en) * | 2014-05-27 | 2014-08-20 | 安徽大地熊新材料股份有限公司 | Method for preparing anti-corrosion wear-resisting sintered Nd-Fe-B magnets |
| 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 |
| 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 |
| CN109103010B (en) * | 2018-08-02 | 2021-05-18 | 浙江东睦科达磁电有限公司 | Material and method for improving density of magnetic powder core insulating layer |
| CN109097810A (en) * | 2018-08-06 | 2018-12-28 | 佛山科学技术学院 | A kind of phosphating process of the phosphate coating for neodymium iron boron surface |
| CN109137004B (en) * | 2018-10-17 | 2020-10-16 | 天津京磁电子元件制造有限公司 | Method for electroplating nickel, copper and nickel on sintered neodymium-iron-boron magnet |
| CN110983416A (en) * | 2019-12-31 | 2020-04-10 | 枣阳市旺前电泳涂料有限公司 | Electrophoretic paint painting process |
| CN115595572A (en) * | 2022-06-10 | 2023-01-13 | 扬州保来得科技实业有限公司（Cn） | Method for improving corrosion resistance of powder metallurgy iron substrate |
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