CN1807686A - Surface anti-rust treatment method for powder moulded permanent magnet - Google Patents
Surface anti-rust treatment method for powder moulded permanent magnet Download PDFInfo
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- CN1807686A CN1807686A CN 200610049511 CN200610049511A CN1807686A CN 1807686 A CN1807686 A CN 1807686A CN 200610049511 CN200610049511 CN 200610049511 CN 200610049511 A CN200610049511 A CN 200610049511A CN 1807686 A CN1807686 A CN 1807686A
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Abstract
The invention discloses a surface rust prevention treatment method of covered powder forming permanent magnet, wherein the craft step comprises the following: surface cleaning, vacuum desiccation, dry method for plating membrane and wet method for plating. The method comprises the following steps: proceeding organic solvent surface cleaning and vacuum desiccation of powder forming permanent magnet surface; carrying on surface vacuum sputtering; evaporating one deck anti-rust metal; entering acid nickel-plated liquor to carry on surface chemistry plating or plating method. The method overcomes etching residual liquid of plating with wet method, which accomplishes long-term rust-resisting of permanent magnet.
Description
Technical field
The invention belongs to the technical field of the antirust processing of metal material surface, particularly relate to a kind of surface anti-rust treatment method for powder moulded permanent magnet that adopts the dry vacuum plating to add the wet method lining.
Background technology
Powder moulded permanent magnet has very high magnetic energy product, in fields such as motor, electroacoustic, instrument, microwave, computer, automotive industrys purposes is widely arranged, it is one of stay material of hyundai electronics industry, China is permanent magnet big producing country, output occupies first place in the world, and wherein only the output in Zhejiang Province just reaches 1/3 of world wide production.Powder moulded permanent magnet is that the permanent magnet of powder compacting contains a lot of holes by the acquisition of magnetizing after powder sintered or the powder bonded moulding.The erosion resistance of permanent magnet own is very poor, if permanent magnet does not carry out antirust processing at once after the general moulding, the aqueous vapor in the atmosphere will soon be corroded magnet.At present powder moulded permanent magnet generally adopts after the moulding directly with wet method antirusting treating methods such as electroless plating or plating, by the approaching millimeter of a wet method lining thickness rustproof layer, to obtain the antirust ability of permanent magnet, but in wet method lining process, plating bath has very strong corrosion and infiltration to become raffinate to porous crack magnet, become " source " of early stage corrosion, directly cause the permanent magnet rustproof layer bonding force of powder compacting poor, early stage peeling comes off, long-term resistant to tarnishing ability is low.For example adopt the magnet of electroless plating or 0.5 millimeter rustproof layer of electronickelling, salt-fog test preferably has only 150-200 hour.Wet method is plated the severe contamination of ubiquity plating bath in addition.The vacuum plating is a kind of new coating technique that rises in recent years, abroad begin one's study at present and adopt the way of vacuum lining permanent magnet rustproof layer, the vacuum plating of dry method can be avoided the corrosion of wet method plating raffinate, but vacuum plating speed is plated well below wet method, no matter be vacuum-evaporation or vacuum sputtering, the anti-rust film that obtains nearly millimeter thickness hardly may because on the one hand the lining time look unactual, blocked up on the one hand rete unrelieved stress is very big, bonding force is low on the contrary.If reduce the rustproof layer thickness of vacuum plating, then be not enough to stop the scattering and permeating corrosion of extraneous aqueous vapor etc.Therefore, the long-term resistant to tarnishing ability that how to realize permanent magnet is the problem that people pay close attention to and study always.
Summary of the invention
The object of the invention provides simple, the no long surface anti-rust treatment method for powder moulded permanent magnet of raffinate burn into resistant to tarnishing time of a kind of technology.
The present invention adopts such technical solution to realize, its processing step is surface cleaning, vacuum-drying, dry method plating counterdie and wet method plated film; Its concrete operation thes contents are as follows:
1, surface cleaning: the permanent magnet of powder compacting is put into the ultrasonic cleaning of organic solvent normal temperature, scavenging period is to remove greasy dirt in 10～30 minutes, wherein organic solvent be purity more than 95%, moisture be lower than 1% have molecular polarity, a volatile organic solvent;
Described organic solvent is a kind of in acetone, the tetracol phenixin equal solvent, and the permanent magnet surfaces of powder compacting does not have the residual of corrosive liquid after cleaning, and reaches the cleaning requirement before the lining;
2, vacuum-drying: the permanent magnet after will cleaning is placed on rapidly in the vacuum coater, be evacuated to vacuum tightness 1～10Pa after, stopped 10～30 minutes, to drain liquid solvent residual in the permanent magnet hole;
3, dry method plating counterdie: dried permanent magnet is put into vacuum coater, be evacuated to local vacuum tightness 10
-3Behind the Pa order of magnitude, adopt the permanent magnet surfaces lining layer of metal film of dry method lining technology in cleaning, this metal bottom film thickness is between 1 micron-100 microns, and its standard potential is less than iron standard potential-0.037V;
The making material of described metal counterdie is a kind of in aluminium, zinc, the nickel etc.;
Described dry method lining is meant a kind of in vacuum-evaporation, evaporated ions plating, d.c. sputtering, radio-frequency sputtering and the intermediate frequency sputter coating;
4, wet method plated film: the permanent magnet behind the dry method plated film is put into acid chemical plating nickel solution carry out wet method lining nickel; adopt a kind of technology in known acid liquefaction nickel plating or the electronickelling; on the basis of metal counterdie, plate the layer of surface metallic membrane again; this thickness of metal film plays the uncorroded effect of protection permanent magnet between 1 micron～10 millimeters.
Compared with prior art, because the present invention has adopted the technology of dry vacuum lining metal counterdie and the multiple metal-coated membrane of wet method, thereby can seal and clog the magnet surface microporosity, it has not only overcome the corrosion of wet method plating raffinate, has avoided retaining between coating and matrix in the wet method lining possibility of inclusion simultaneously; And the membranous layer binding force of dry vacuum plating is good, and the bottoming of this layer transition layer is arranged between magnet and wet method coating, can effectively improve membranous layer binding force, and underlying membrane adopts electropotential to be higher than the metallic substance of iron, can also play the effect of anodic protection.
Description of drawings
Rustproof layer and powder moulded permanent magnet cross section structure synoptic diagram that Fig. 1 makes for the inventive method
Drawing reference numeral explanation: 1-permanent magnet, 2-metal counterdie, 3-metal film on surface.
Embodiment
Surface anti-rust treatment method for powder moulded permanent magnet of the present invention, it is to adopt surface cleaning, vacuum-drying, dry method plating counterdie and wet method coating process step to realize, is described further below by specific embodiment:
Embodiment 1:
Surface cleaning: the permanent magnet of powder compacting is put into purity more than 95%, moisturely is lower than 1% acetone ultrasonic cleaning after 20 minutes, take out, the permanent magnet surfaces of cleaning the back powder compacting does not have the residual of corrosive liquid, reaches the cleaning requirement before the lining;
Vacuum-drying: the permanent magnet after will cleaning is placed on rapidly in the vacuum plating cavity, change the sputtering target in the vacuum plating cavity into the aluminium target, 12 centimetres of target sheet spacings are evacuated to vacuum tightness to 5Pa, stopped 30 minutes, to drain liquid solvent residual in the permanent magnet hole;
Dry method plating counterdie: dried permanent magnet is put into vacuum coater, be evacuated to local vacuum tightness 5 * 10
-3Behind the Pa, charge into argon gas to vacuum tightness 0.5Pa, and be stabilized in this vacuum tightness, open shielding power supply, feed-in power density 20W/cm
2, the planet horse rotates, and opens baffle plate after stablizing and begins d.c. sputtering, behind the aluminium film of 5 microns of magnet surface lining one layer thicknesses, kept in a vacuum 30 minutes after 30 minutes, reduce the temperature rise that surface sputtering produces, put into atmosphere again and open vacuum cavity, take out the good magnet of lining; The standard potential of described aluminium film is less than iron standard potential-0.037V, aluminium film can form the anodic protection metal in magnet surface, insert and seal the hole of porous magnet simultaneously,, can avoid wet method plating bath subsequently to infiltrate magnet with the bottoming of this layer protective membrane;
The wet method plated film: the magnet that the sputter lining is good is put into acid chemical plating nickel solution and is carried out chemical nickel plating; the complex plating process parameter is: acid liquid formula for chemical plating nickel is single nickel salt 25g/L; Trisodium Citrate 15g/L; sodium acetate 13g/L; thiocarbamide 2ppm; inferior sodium phosphate 20g/L; keep 90～95 ℃ of pH value 4.5～4.8 and bath temperatures in the lining; 5～7 microns/minute of lining speed; after 60 minutes; take out magnet water flushing back oven dry; can obtain on the basis of metal counterdie, plating again the permanent magnet of layer of surface metallic nickel film; this metallic nickel film thickness is 1 micron～10 microns, plays the uncorroded effect of protection permanent magnet.
Test according to national standard:
(1) through the normal temperature weathering resistance salt-fog test of 5% sodium-chlor, do not see corrosion after 700 hours;
(2) 25 ℃ and 100 ℃ are thermal shock experiment 20 times repeatedly, does not see that peeling comes off;
(3) normal temperature solution wetted method (10% sodium-chlor+2% gelatin solution) is measured, and rete is not seen blue spot and Cavitations, and the rete densification is described;
(4) standard tension instrumentation examination membranous layer binding force is greater than 8MPa.
Experimental result shows: rete not only has good bonding force, and rete and matrix bond are firm, the even film layer densification, and weathering resistance 700 hours obviously is better than general direct chemical nickel plating magnet 100～200 hours.
Surface cleaning: the permanent magnet of powder compacting is put into purity more than 95%, moisturely is lower than 1% tetracol phenixin ultrasonic cleaning after 20 minutes, take out, the permanent magnet surfaces of cleaning the back powder compacting does not have the residual of corrosive liquid, reaches the preceding cleaning requirement of lining;
Permanent magnet after cleaning is placed on rapidly in the vacuum plating cavity, with in the vacuum plating cavity
Vacuum-drying: the permanent magnet after will cleaning is placed on rapidly in the vacuum plating cavity, to put into commercially pure spelter in the thermal resistance evaporation boat in the vacuum plating cavity, 8 centimetres of target sheet spacings are evacuated to vacuum tightness to 5Pa, stopped 30 minutes, to drain liquid solvent residual in the permanent magnet hole;
Dry method plating counterdie: dried permanent magnet is put into vacuum coater, be evacuated to local vacuum tightness 2 * 10
-3Behind the pa, open the evaporation power supply, electric current is opened baffle plate after slowly being adjusted to 200A, the planet horse rotates, evaporated 10 minutes, and behind the zinc of 12 microns of magnet surface lining one layer thicknesses, kept in a vacuum and reduced the temperature rise that surface evaporation produces in 30 minutes, put into atmosphere and open vacuum cavity, take out the magnet of the good zinc film of lining; The standard potential of described aluminium film is less than iron standard potential-0.037V, aluminium film can form the anodic protection metal in magnet surface, insert and seal the hole of porous magnet simultaneously,, can avoid wet method plating bath subsequently to infiltrate magnet with the bottoming of this layer protective membrane;
The wet method plated film: the magnet that the sputter lining is good is put into acid chemical plating nickel solution and is carried out chemical nickel plating; the complex plating process parameter is: acid liquid formula for chemical plating nickel is single nickel salt 25g/L; Trisodium Citrate 15g/L; sodium acetate 13g/L; thiocarbamide 2ppm; inferior sodium phosphate 20g/L; keep 90～95 ℃ of pH value 4.5～4.8 and bath temperatures in the lining; 5～7 microns/minute of lining speed; after 60 minutes; take out magnet water flushing back oven dry; can obtain on the basis of metal counterdie, plating again the permanent magnet of layer of surface metallic nickel film; this metallic nickel film thickness is 1 micron～10 microns, plays the uncorroded effect of protection permanent magnet.
Test according to national standard:
(1) through the normal temperature weathering resistance salt-fog test of 5% sodium-chlor, do not see corrosion after 600 hours;
(2) 25 ℃ and 100 ℃ are thermal shock experiment 20 times repeatedly, does not see that peeling comes off;
(3) normal temperature solution wetted method (10% sodium-chlor+2% gelatin solution) is measured, and rete is not seen blue spot and Cavitations, and the rete densification is described;
(4) standard tension instrumentation examination membranous layer binding force is greater than 7.5MPa.
Experimental result shows: rete not only has good bonding force, and rete and matrix bond are firm, the even film layer densification, and weathering resistance (600 hours) obviously is better than general direct chemical nickel plating magnet (100～200 hours).
Claims (5)
1, surface anti-rust treatment method for powder moulded permanent magnet, its processing step are surface cleaning, vacuum-drying, dry method plating counterdie and wet method plated film.
2, surface anti-rust treatment method for powder moulded permanent magnet according to claim 1 is characterized in that the concrete operation of described surface cleaning, vacuum-drying, dry method plating counterdie and wet method plated film thes contents are as follows:
Surface cleaning: the permanent magnet of powder compacting is put into the ultrasonic cleaning of organic solvent normal temperature, and scavenging period is to remove greasy dirt in 10～30 minutes, wherein organic solvent be purity more than 95%, moisture be lower than 1% have molecular polarity, a volatile organic solvent; The permanent magnet surfaces of powder compacting does not have the residual of corrosive liquid after cleaning, and reaches the preceding cleaning requirement of lining;
Vacuum-drying: the permanent magnet after will cleaning is placed on rapidly in the vacuum coater, be evacuated to vacuum tightness 1～10Pa after, stopped 10～30 minutes, to drain liquid solvent residual in the permanent magnet hole;
Dry method plating counterdie: dried permanent magnet is put into vacuum coater, be evacuated to local vacuum tightness 10
-3Behind the Pa order of magnitude, adopt the permanent magnet surfaces lining layer of metal film of dry method lining technology in cleaning, this metal bottom film thickness is between 1 micron-100 microns, and its standard potential is less than iron standard potential-0.037V;
Wet method plated film: the permanent magnet behind the dry method plated film is put into acid chemical plating nickel solution carry out wet method lining nickel; adopt a kind of technology in known acid liquefaction nickel plating or the electronickelling; on the basis of metal counterdie, plate the layer of surface metallic membrane again; this thickness of metal film plays the uncorroded effect of protection permanent magnet between 1 micron～10 millimeters.
3, surface anti-rust treatment method for powder moulded permanent magnet according to claim 2 is characterized in that described organic solvent is a kind of in acetone, the tetracol phenixin equal solvent.
4, surface anti-rust treatment method for powder moulded permanent magnet according to claim 2, the making material that it is characterized in that described metal counterdie are a kind of in aluminium, zinc, the nickel etc.
5, surface anti-rust treatment method for powder moulded permanent magnet according to claim 2 is characterized in that described dry method lining is meant a kind of in vacuum-evaporation, evaporated ions plating, d.c. sputtering, radio-frequency sputtering and the intermediate frequency sputter coating.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173763A (en) * | 2013-03-28 | 2013-06-26 | 宁波韵升股份有限公司 | Electroplating and vapor deposition composite protection method for neodymium-iron-boron magnet |
| CN110699635A (en) * | 2019-10-12 | 2020-01-17 | 宁波慧钜鑫新材料科技有限公司 | Sintered NdFeB surface plasma synergistic vapor deposition Ni material and preparation process |
| CN110983334A (en) * | 2019-12-18 | 2020-04-10 | 宁波韵升股份有限公司 | Neodymium-iron-boron magnet composite nickel plating method |
| CN111411380A (en) * | 2020-04-15 | 2020-07-14 | 安徽大地熊新材料股份有限公司 | Electroplating process |
| CN111826687A (en) * | 2020-07-07 | 2020-10-27 | 曲靖中铭科技有限公司 | Processing technology of surface coating of stainless steel MIM product |
| CN112002514A (en) * | 2020-08-25 | 2020-11-27 | 成都银磁材料有限公司 | Injection molding magnet and preparation method thereof |
| CN112071612A (en) * | 2020-08-11 | 2020-12-11 | 宁波金科磁业有限公司 | Neodymium-iron-boron magnet and preparation method thereof |
-
2006
- 2006-02-16 CN CN 200610049511 patent/CN1807686A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173763A (en) * | 2013-03-28 | 2013-06-26 | 宁波韵升股份有限公司 | Electroplating and vapor deposition composite protection method for neodymium-iron-boron magnet |
| CN110699635A (en) * | 2019-10-12 | 2020-01-17 | 宁波慧钜鑫新材料科技有限公司 | Sintered NdFeB surface plasma synergistic vapor deposition Ni material and preparation process |
| CN110983334A (en) * | 2019-12-18 | 2020-04-10 | 宁波韵升股份有限公司 | Neodymium-iron-boron magnet composite nickel plating method |
| CN111411380A (en) * | 2020-04-15 | 2020-07-14 | 安徽大地熊新材料股份有限公司 | Electroplating process |
| CN111826687A (en) * | 2020-07-07 | 2020-10-27 | 曲靖中铭科技有限公司 | Processing technology of surface coating of stainless steel MIM product |
| CN112071612A (en) * | 2020-08-11 | 2020-12-11 | 宁波金科磁业有限公司 | Neodymium-iron-boron magnet and preparation method thereof |
| CN112002514A (en) * | 2020-08-25 | 2020-11-27 | 成都银磁材料有限公司 | Injection molding magnet and preparation method thereof |
| CN112002514B (en) * | 2020-08-25 | 2022-04-01 | 成都银磁材料有限公司 | Injection molding magnet and preparation method thereof |
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