CN107039168B - A kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating - Google Patents

A kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating Download PDF

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Publication number
CN107039168B
CN107039168B CN201710282805.3A CN201710282805A CN107039168B CN 107039168 B CN107039168 B CN 107039168B CN 201710282805 A CN201710282805 A CN 201710282805A CN 107039168 B CN107039168 B CN 107039168B
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rare
permanent magnet
earth permanent
plating
electroplating
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CN107039168A (en
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裴文利
田昂
吴文远
温权
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Liangshan Rare Earth Industry Technology Research Institute
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Liangshan Rare Earth Industry Technology Research Institute
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/026Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/20Electroplating using ultrasonics, vibrations
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
    • C25D5/36Pretreatment of metallic surfaces to be electroplated of iron or steel
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/001Magnets

Abstract

The invention belongs to corrosion resistant surfaces processing technology field, in particular to a kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating.Then the present invention carries out Fe-B rare-earth permanent magnet vacuumize process first to Fe-B rare-earth permanent magnet surface preparation, be finally electroplated using electroplating in ultrasonic field slot.The invention avoids coating caused by liberation of hydrogen effect to play drum, blistering, improves the antiseptic property of Fe-B rare-earth permanent magnet surface covering, is expected to substitute existing neodymium iron boron electroplating anticorrosion technology, therefore have boundless application prospect.

Description

A kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating
Technical field
The invention belongs to corrosion resistant surfaces processing technology field, in particular to a kind of Fe-B rare-earth permanent magnet electroplating surface applies The preparation method of layer.
Background technique
Fe-B rare-earth permanent magnet is more and more applied with its excellent magnetic property, is widely used in automobile electricity It is mechanical, electrical ladder motor, energy-saving electric machine, medical treatment Magnetic resonance imaging, computer hard disc driver, the vibrating motor of mobile phone, sound equipment, The motor of hybrid vehicle, wind-driven generator etc..
Since Fe-B rare-earth permanent magnet is oxidizable, it is general in the use of above-mentioned Fe-B rare-earth permanent magnet all need to be into Row surface coated treatment.The coating method being widely used at present mainly be electroplated, on neodymium iron boron matrix electrogalvanizing, electronickelling, Electronickelling cupro-nickel etc..However neodymium iron boron magnetic body is usually that powder metallurgical technique is used to prepare, therefore the matrix and metal of magnet Material is compared, loose porous, contains a large amount of micropore.Liberation of hydrogen effect, the hydrogen of generation are had in pre-electroplating treatment and electroplating process It can penetrate into, be adsorbed in the micropore of matrix surface, after this matrix surface for seeping hydrogen or inhaling hydrogen plates one layer of coating, when covering is plated When layer ambient temperature increases, the hydrogen of absorption can be excessive because expanding, and generates a kind of pressure to coating, so that coating is detached from matrix and convex It rises, has formed drum, blistering, caused coating to fail, seriously affect the anti-corrosion ability of coating.Since neodymium iron boron matrix surface contains greatly Amount micropore, it is loose be preparation process determine, and liberation of hydrogen effect be also in electroplating process inevitably, therefore at present rare earth forever The electroplating quality of magnet always can not be compared with common metal matrix electroplating quality, this disadvantage also seriously constrains it in electricity It further applies in the fields such as mechanical, electrical son, aerospace.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of system of Fe-B rare-earth permanent magnet electroplating surface coating Preparation Method, it is therefore an objective to avoid coating caused by liberation of hydrogen effect from playing drum, blistering, improve the anti-of Fe-B rare-earth permanent magnet surface covering Rotten performance.
The preparation method of Fe-B rare-earth permanent magnet electroplating surface coating of the invention, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
When Fe-B rare-earth permanent magnet volume is less than 0.5cm3When, oil removing and acid are carried out to Fe-B rare-earth permanent magnet surface It washes;
When Fe-B rare-earth permanent magnet volume is greater than 1cm3When, sandblasting is carried out to Fe-B rare-earth permanent magnet surface;
When Fe-B rare-earth permanent magnet volume is in 0.5 ~ cm3Between when, carry out oil removing and pickling or sandblasting;
Wherein, the oil removing is on Fe-B rare-earth permanent magnet surface, using the oil removing at 40 ~ 80 DEG C of metal cleaning solution 5~60min;Pickling be use pH value for 1 ~ 5 dilute sulfuric acid or dilute hydrochloric acid, 1 ~ 120s of pickling, then at room temperature ~ 100 DEG C do It is dry;
The sandblasting is to use spray gun that granularity is sprayed onto Fe-B rare-earth permanent magnet surface for the fine sand of 400 ~ 1000 mesh, The oxide layer of magnet surface is removed, until exposing linen fresh surface;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, electroplating in ultrasonic field slot be Trench bottom is electroplated, ultrasonic wave generating box is installed, plating uses barrel plating technique or rack plating process;
Wherein, the barrel plating technique detailed process is:
(a) Fe-B rare-earth permanent magnet after vacuumize process is fitted into electro-plating roller, and mixes steel ball as filler, Electro-plating roller is put into electroplating in ultrasonic field slot;
(b) rotating cylinder revolving speed is 5-60 rpm, opens ultrasonic wave generating box power supply and electroplating power supply, starts to be rolled Plating;
(c) bath temperature control is at 35-50 DEG C during barrel plating, and pH value controls between 1-6, and barrel plating 5-120 min is obtained To the Fe-B rare-earth permanent magnet electroplating surface coating with a thickness of 0.1 ~ 40 μm;
The rack plating process detailed process is:
(a) volume is greater than 2 cm3Vacuumize process after Fe-B rare-earth permanent magnet be put on rack plating frame, after clipping It is put into electroplating in ultrasonic field slot;
(b) ultrasonic wave generating box power supply and electroplating power supply are opened, starts to carry out rack plating;
(c) bath temperature control is at 35-50 DEG C, and pH value controls between 2 and 6, rack plating 5-120 min, be made with a thickness of The Fe-B rare-earth permanent magnet electroplating surface coating of 0.1 ~ 40 μm of 0.1 ~ 40 μm.
Wherein, the spray painting pressure of the spray gun is 1 ~ 15MPa.
In the electro-plating roller by volume, Fe-B rare-earth permanent magnet: steel ball=(1 ~ 10): 4, the diameter of steel ball is 0.1~1cm。
The plating solution is business Ni, Cu or Zn plating solution, and the electroplated coating is Ni, Cu, Zn coating or Ni-Cu-Ni Composite deposite first carries out barrel plating or rack plating in Ni bath trough, is being transferred to Cu plating solution when preparing Ni-Cu-Ni composite deposite Slot carries out barrel plating or rack plating, eventually passes back to carry out barrel plating or rack plating in Ni bath trough.
A kind of preparation method of Fe-B rare-earth permanent magnet surface metal electroplated coating of the present invention, has the following characteristics that
(1) since neodymium iron boron matrix contains a large amount of micropore, in these micropores in pretreatment process, hydrogen aggregation is had, Or have air residual, it causes the residual of micro-porous area cannot exclude in plating stage, will lead to air and hydrogen remains in micropore Interior, inside coating, once outside temperature increases, gas expansion makes coating play drum, blistering, or even cracking, influences the anti-corrosion of coating Performance.The present invention increases the vacuumize process of neodymium iron boron matrix after pretreatment process, and vacuum reaches 10-1Pa is hereinafter, by neodymium Hydrogen extraction in iron boryl body micropore, avoids workpiece and contains air and hydrogen in micropore before immersing electroplating bath;
(2) it is easy to produce liberation of hydrogen effect in electroplating process, these hydrogen being precipitated can be gathered in the micropore of matrix, after plating Remain in inside coating, once outside temperature increases, gas expansion makes coating play drum, blistering, or even cracking, influences coating Antiseptic property.The present invention introduces ultrasonic wave in the plating process, due to the airburst effect of ultrasonic wave, the hydrogen in micropore can be shaken Out, it avoids hydrogen from assembling in micropore, liberation of hydrogen effect can effectively be avoided to play drum, blistering or even problem of Cracking to coating bring;
(3) simultaneously as the effect of ultrasonic wave, in plating solution infiltration into microporous, micro-porous area can also plate coating, increase The bonded area of coating and matrix, therefore the binding force of coating is improved, to obtain high quality, closely knit anti-corrosion coating;
(4) the energy effect of ultrasonic wave, keeps solution composition, pH value, temperature in bath trough etc. more uniform, leads to plating piece Surrounding current density is almost the same, and coating can be made to deposit more evenly in matrix surface, reduce the wall and corner effect of Common platings, Avoid the blocked up disadvantage of corner coating.
For the present invention compared with existing electroplating technology, advantage is it will be evident that showing themselves in that
(1) hydrogen in neodymium iron boron matrix micropore is extracted out, is avoided using the workpiece before vacuumize process plating by the present invention Workpiece contains air and hydrogen before immersing electroplating bath in micropore, reduce hydrogen remaining probability in micropore after plating;
(2) introducing ultrasonic wave can due to the airburst effect of ultrasonic wave as supplementary means in the plating process by the present invention The hydrogen that liberation of hydrogen effect generates will be electroplated to shake from micropore out, and be discharged outside plating solution, avoid hydrogen from assembling in micropore, can effectively keep away Exempt from liberation of hydrogen effect and drum, blistering or even problem of Cracking are risen to coating bring;
(3) due to the effect of ultrasonic wave, plating solution is improved to the wetting ability of micropore, plating solution can be micro- in infiltration into microporous Bore region can also plate coating, increase the bonded area of coating and matrix, therefore improve the binding force of coating, to obtain High quality, closely knit anti-corrosion coating are obtained, the anti-corrosion ability on Fe-B rare-earth permanent magnet surface is significantly improved, prolongs the service life;
(4) the vibration stirring action of ultrasonic wave keeps solution composition, pH value, temperature in bath trough etc. more uniform, causes Current density is almost the same around plating piece, and coating can be made to deposit more evenly in matrix surface, reduce the corner of Common platings Effect avoids the blocked up disadvantage of corner coating;
(5) all there is important application in fields such as electronics, information, motor, aviation, navigation, space flight due to neodymium iron boron magnetic body, The present invention is expected to substitute existing neodymium iron boron electroplating anticorrosion technology, therefore has boundless application prospect.
Detailed description of the invention
Fig. 1 is Fe-B rare-earth permanent magnet vacuumize process schematic diagram in the present invention;
Wherein: 1: sealed tank cap;2: sealing can body;3: vacuum-pumping tube valve;4: vacuum-pumping tube;5: electroplate liquid access tube Valve;6: electroplate liquid access tube;
Fig. 2 is electroplating in ultrasonic field slot schematic diagram of the present invention;
Wherein: 7: ultrasonic wave generating box;8: electroplating bath;
Fig. 3 is the concrete structure schematic diagram of ultrasonic wave generating box in Fig. 2;
Wherein: 9: ultrasonic transducer;10: titanium shell;
Fig. 4 is that Zn layers and coating appearance comparison diagram in embodiment 1 are commercially plated in the embodiment of the present invention 8;
Wherein: Zn layers A: are plated in embodiment;B: Zn layers of business plating.
Specific embodiment
The plating metal coating Preparation equipment used in the embodiment of the present invention is as shown in Figure 1, Figure 2 and Figure 3, further includes barrel plating Roller or rack plating hanger.
Electroplating bath involved in the embodiment of the present invention, rotating plating cylinder, rack plating hanger belong to business equipment, can be from market Purchase;Hermetically sealed can in Fig. 1 is home-built equipment, and anticorrosive PTFE layer, sealing are coated in the metal bucket that diameter is 500mm There are vacuum meter and two to be passed through the pipeline of tube valve 5 with vacuum-pumping tube valve 3 and electroplate liquid on cover 1, wherein vacuum-pumping tube 4 It is connected with vacuum mechanical pump, electroplate liquid access tube 6 is connected with the plating liquid case prepared;
Electroplating in ultrasonic field slot is as shown in Figures 2 and 3, is home-built equipment, several ultrasonic transducers 9 is welded to certain On the Ti plate of size, weld transducing head quantity and Ti board size it is related with the power of ultrasonic transducer, usually compared with electroplating bath Relatively high power generator is selected, selecting power principle is the plating solution surface layer that ultrasonic wave can shake electroplating bath, then uses Welder Energy converter is coated in the box i.e. titanium shell 10 of Ti plate welding by skill, and the electric wire being connected with energy converter is reserved by titanium shell 10 Hole draw, hole hole is sealed up using polytetrafluoroethylene (PTFE), prevents plating solution from penetrating into.
The Fe-B rare-earth permanent magnet used in the embodiment of the present invention is bought for business magnet from market, and the magnet trade mark is 40SH。
Embodiment 1
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
Sandblasting is carried out to having a size of 30mm × 30mm × 3mm Fe-B rare-earth permanent magnet surface, using spray gun by granularity It is sprayed onto Fe-B rare-earth permanent magnet surface for the fine sand of 400 ~ 1000 mesh, the oxide layer of magnet surface is removed, exposes canescence Fresh surface until;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses rack plating work Fe-B rare-earth permanent magnet is put on rack plating frame by skill, is put into electroplating in ultrasonic field slot after clipping, and ultrasonic transducer electricity is opened Source and electroplating power supply start to carry out rack plating, and plating solution is business Zn plating solution, and temperature control is at 40 DEG C, pH value 4,120 min of rack plating, The Fe-B rare-earth permanent magnet surface Zn coating with a thickness of 20 μm is made.
Embodiment 2
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
Sandblasting is carried out to having a size of 40mm × 20mm × 3mm Fe-B rare-earth permanent magnet surface, using spray gun by granularity It is sprayed onto Fe-B rare-earth permanent magnet surface for the fine sand of 400 ~ 1000 mesh, the oxide layer of magnet surface is removed, exposes canescence Fresh surface until;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses rack plating work Fe-B rare-earth permanent magnet is put on rack plating frame by skill, is put into electroplating in ultrasonic field slot after clipping, and ultrasonic transducer electricity is opened Source and electroplating power supply start to carry out rack plating, and plating solution is business Ni plating solution, and at 45 DEG C, pH value 5,40 min of rack plating is made for temperature control Obtain the Fe-B rare-earth permanent magnet surface Ni coating with a thickness of 8 μm.
Embodiment 3
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
Sandblasting is carried out to having a size of 20mm × 20mm × 10mm Fe-B rare-earth permanent magnet surface, using spray gun by granularity It is sprayed onto Fe-B rare-earth permanent magnet surface for the fine sand of 400 ~ 1000 mesh, the oxide layer of magnet surface is removed, exposes canescence Fresh surface until;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses rack plating work Fe-B rare-earth permanent magnet is put on rack plating frame by skill, is put into electroplating in ultrasonic field slot after clipping, and ultrasonic transducer electricity is opened Source and electroplating power supply start to carry out rack plating, and plating solution is business Ni plating solution, and temperature control is at 35 DEG C, and pH value 2,20 min of rack plating will Hanger taking-up is put into business Cu bath trough, pH value 3, and temperature is 42 DEG C, is electroplated 10 minutes, then pendant taking-up is put into business In Ni bath trough, pH value 4, temperature is 42 DEG C, is electroplated 30 minutes, and the Ni-Cu-Ni electroplated coating with a thickness of 10 μm is made.
Embodiment 4
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
Carry out oil removing and pickling to having a size of 10mm × 10mm × 3mm Fe-B rare-earth permanent magnet surface, oil removing be Fe-B rare-earth permanent magnet surface, using metal cleaning solution at 40 DEG C oil removing 30min;Pickling be use pH value for 2 dilute sulphur Acid, pickling 100s are then dry at 25 DEG C of room temperature;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses barrel plating work Fe-B rare-earth permanent magnet is put into roller by skill, is used as and is filled out according to magnet and packing volume ratio 1:2 addition diameter 5mm steel ball Material, roller is put into electroplating in ultrasonic field slot, opens ultrasonic transducer power supply and electroplating power supply, starts to carry out barrel plating, plating solution For business Ni plating solution, at 38 DEG C, roller taking-up is put into business Cu bath trough, pH by pH value 2,120 min of barrel plating for temperature control Value is 3, and temperature is 42 DEG C, is electroplated 20 minutes, then pendant taking-up is put into business Ni bath trough, pH value 5, temperature 40 DEG C, it is electroplated 30 minutes, the Ni-Cu-Ni electroplated coating with a thickness of 11 μm is made.
Embodiment 5
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
Carry out oil removing and pickling to having a size of 20mm × 10mm × 3mm Fe-B rare-earth permanent magnet surface, oil removing be Fe-B rare-earth permanent magnet surface, using metal cleaning solution at 80 DEG C oil removing 5min;Pickling be use pH value for 1 dilute salt Acid, pickling 10s are then dry at 50 DEG C;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses barrel plating work Fe-B rare-earth permanent magnet is put into roller by skill, is used as and is filled out according to magnet and packing volume ratio 1:1 addition diameter 10mm steel ball Material, roller is put into electroplating in ultrasonic field slot, opens ultrasonic transducer power supply and electroplating power supply, starts to carry out barrel plating, plating solution For business Ni plating solution, at 45 DEG C, the Ni electroplated coating with a thickness of 15 μm is made in pH value 6,120 min of barrel plating for temperature control.
Embodiment 6
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
It is in neodymium to oil removing and pickling, oil removing is carried out having a size of 5mm × 5mm × 5mm Fe-B rare-earth permanent magnet surface Iron boron rare-earth permanent magnet surface, using metal cleaning solution at 40 DEG C oil removing 60min;Pickling be use pH value for 5 dilute sulfuric acid, Pickling 120s is then dry at 100 DEG C;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses barrel plating work Fe-B rare-earth permanent magnet is put into roller by skill, is used as and is filled out according to magnet and packing volume ratio 1:4 addition diameter 1mm steel ball Material, roller is put into electroplating in ultrasonic field slot, opens ultrasonic transducer power supply and electroplating power supply, starts to carry out barrel plating, plating solution For business Zn plating solution, at 41 DEG C, the Zn electroplated coating with a thickness of 12 μm is made in pH value 5.5,60 min of barrel plating for temperature control.
Embodiment 7
The preparation method of the Fe-B rare-earth permanent magnet electroplating surface coating of the present embodiment, follows the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
Carry out oil removing and pickling to having a size of 15mm × 10mm × 3mm Fe-B rare-earth permanent magnet surface, oil removing be Fe-B rare-earth permanent magnet surface, using metal cleaning solution at 60 DEG C oil removing 20min;Pickling be use pH value for 3 dilute salt Acid, pickling 80s are then dry at 30 DEG C;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) is surrounded by inside hermetically sealed can Coating, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and plating on sealed tank cap Valve is designed on liquid access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve opened on vacuum-pumping tube carries out It is evacuated to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, to sealing It is passed through electroplate liquid in tank, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, then takes out Fe-B rare-earth permanent magnet It is electroplated at once;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and plating uses barrel plating work Fe-B rare-earth permanent magnet is put into roller by skill, is used as and is filled out according to magnet and packing volume ratio 1:1 addition diameter 8mm steel ball Material, roller is put into electroplating in ultrasonic field slot, opens ultrasonic transducer power supply and electroplating power supply, starts to carry out barrel plating, plating solution For business Ni plating solution, at 40 DEG C, roller taking-up is put into business Cu bath trough, pH by pH value 3,120 min of barrel plating for temperature control Value is 4.5, and temperature is 42 DEG C, is electroplated 60 minutes, then roller taking-up is put into business Ni bath trough, pH value 5, temperature 40 DEG C, it is electroplated 60 minutes, the Ni-Cu-Ni electroplated coating with a thickness of 20 μm is made.
Embodiment 8
There is Zn coating Fe-B rare-earth permanent magnet and embodiment 2 to prepare the surface of 1 electroplating in ultrasonic field of embodiment preparation Electroplating in ultrasonic field preparation surface have Ni-Cu-Ni coating Fe-B rare-earth permanent magnet and purchase business plating Zn and NiCuNi layers of magnet, it is common to carry out neutral salt spray test and PCT test.
The present embodiment neutral salt spray test condition are as follows: 5% NaCl solution, temperature are 35 DEG C, and splash speed is 1.5ml/ Hr, pH=6.5 ~ 7.2;PCT test condition are as follows: 120 DEG C, 100% humidity, in 2.0 atmospheric pressures.
The corrosion condition for observing sample, the testing time of the sample is recorded when bubble, rust spot occurs in sample, which makees For the anti-corrosion time of the sample.Test result is as shown in table 1:
The comparison of serial number 2 and serial number 4 is as shown in figure 4, it can be seen from above-described embodiment that using neodymium iron boron of the invention The coating of electroplating in ultrasonic field is passed through on rare-earth permanent magnet surface, and white color is bright, and coating surface is fine and smooth, and ordinary plating process preparation Coating surface waviness is larger (as shown in circled in Fig. 4 B), by comparison it is apparent that the present invention is remarkably improved magnetic The corrosion resistance and matrix of body and the binding ability of coating.

Claims (3)

1. a kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating, it is characterised in that follow the steps below:
(1) Fe-B rare-earth permanent magnet surface preparation:
When Fe-B rare-earth permanent magnet volume is less than 0.5cm3When, oil removing and pickling are carried out to Fe-B rare-earth permanent magnet surface;
When Fe-B rare-earth permanent magnet volume is greater than 1cm3When, sandblasting is carried out to Fe-B rare-earth permanent magnet surface;
When Fe-B rare-earth permanent magnet volume is in 0.5~cm3Between when, carry out oil removing and pickling or sandblasting;
Wherein, the oil removing be on Fe-B rare-earth permanent magnet surface, using metal cleaning solution at 40~80 DEG C oil removing 5~ 60min;Pickling be use pH value for 1~5 dilute sulfuric acid or dilute hydrochloric acid, 1~120s of pickling, then at room temperature~100 DEG C do It is dry;
The sandblasting is to use spray gun that granularity is sprayed onto Fe-B rare-earth permanent magnet surface for the fine sand of 400~1000 mesh, will The oxide layer of magnet surface is removed, until exposing linen fresh surface;
(2) Fe-B rare-earth permanent magnet vacuumize process:
Fe-B rare-earth permanent magnet through surface preparation is put into hermetically sealed can, polytetrafluoroethylene (PTFE) painting is surrounded by inside hermetically sealed can Layer, hermetically sealed can top are sealed tank caps, connect vacuum-pumping tube and electroplate liquid access tube, vacuum-pumping tube and electroplate liquid on sealed tank cap Valve is designed on access tube;
After Fe-B rare-earth permanent magnet is put into hermetically sealed can, sealed tank cap is covered, the valve on vacuum-pumping tube is opened and take out very Sky is to vacuum degree 10-1Pa hereinafter, close vacuum-pumping tube on valve, open electroplate liquid access tube on valve, into hermetically sealed can It is passed through electroplate liquid, until Fe-B rare-earth permanent magnet is totally immersed into plating solution, is then taken out Fe-B rare-earth permanent magnet at once It is electroplated;
(3) Fe-B rare-earth permanent magnet electroplating surface: being electroplated using electroplating in ultrasonic field slot, and electroplating in ultrasonic field slot is to be electroplated Trench bottom installs ultrasonic wave generating box, and plating uses barrel plating technique or rack plating process;
Wherein, the barrel plating technique detailed process is:
(a) Fe-B rare-earth permanent magnet after vacuumize process is fitted into electro-plating roller, and mixes steel ball as filler, it will be electric Plating roller is put into electroplating in ultrasonic field slot;
(b) rotating cylinder revolving speed is 5-60rpm, opens ultrasonic wave generating box power supply and electroplating power supply, starts to carry out barrel plating;
(c) bath temperature control is at 35-50 DEG C during barrel plating, and pH value controls between 1-6, and barrel plating 5-120min obtains thickness The Fe-B rare-earth permanent magnet electroplating surface coating that degree is 0.1~40 μm;
The rack plating process detailed process is:
(a) volume is greater than 2cm3Vacuumize process after Fe-B rare-earth permanent magnet be put on rack plating frame, be put into after clipping super In sound wave electroplating bath;
(b) ultrasonic wave generating box power supply and electroplating power supply are opened, starts to carry out rack plating;
(c) at 35-50 DEG C, pH value is controlled between 2 and 6 for bath temperature control, and rack plating 5-120min is made with a thickness of 0.1~40 μm 0.1~40 μm of Fe-B rare-earth permanent magnet electroplating surface coating, the plating solution is business Ni, Cu or Zn plating solution, institute The electroplated coating stated is Ni, Cu, Zn coating or Ni-Cu-Ni composite deposite, when preparing Ni-Cu-Ni composite deposite, first in Ni Barrel plating or rack plating are carried out in bath trough, are carried out barrel plating or rack plating being transferred to Cu bath trough, are eventually passed back to carry out in Ni bath trough Barrel plating or rack plating.
2. a kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating according to claim 1, feature exist In the spray gun spray painting pressure be 1~15MPa.
3. a kind of preparation method of Fe-B rare-earth permanent magnet electroplating surface coating according to claim 1, feature exist In the electro-plating roller by volume, Fe-B rare-earth permanent magnet: steel ball=(1~10): 4, the diameter of steel ball is 0.1~ 1cm。
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