CN109346306A - A kind of In-situ reaction coating and preparation method thereof for neodymium iron boron magnetic body surfacecti proteon - Google Patents
A kind of In-situ reaction coating and preparation method thereof for neodymium iron boron magnetic body surfacecti proteon Download PDFInfo
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- CN109346306A CN109346306A CN201811260774.2A CN201811260774A CN109346306A CN 109346306 A CN109346306 A CN 109346306A CN 201811260774 A CN201811260774 A CN 201811260774A CN 109346306 A CN109346306 A CN 109346306A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
- H01F41/026—Apparatus 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of PM
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/0221—Mounting means for PM, supporting, coating, encapsulating PM
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Abstract
The present invention relates to Nd-Fe-B permanent magnet material, surfacecti proteon and spraying technology fields, a kind of In-situ reaction coating and preparation method thereof for neodymium iron boron magnetic body surfacecti proteon is specifically disclosed, pure aluminum coating is prepared in the magnet surface Jing Guo preceding processing using spraying process；Then surface polishing cleaning and anodized are carried out to pure aluminum coating, prepares aluminum oxide film on pure aluminum coating surface, Nickel acetate sealing processing is carried out to aluminum oxide film later, as a result, prepared by the generated in-situ aluminium of magnet surface/alumina composite coating.Aluminium/aluminium oxide In-situ reaction coating compares more simple aluminized coating, and corrosion resistance is strong, has the advantages such as high-compactness, highly corrosion resistant, higher hardness and higher abrasion resistance；And fitness, binding force and the stability of In-situ reaction coating are also superior to simple Double-layer aluminum-alumina composite coating.
Description
Technical field
The present invention relates to Nd-Fe-B permanent magnet material, surfacecti proteon and spraying technology fields, specifically disclose a kind of use
In the In-situ reaction coating and preparation method thereof of neodymium iron boron magnetic body surfacecti proteon.
Background technique
Nd-Fe-B based permanent magnetic material is the presently found rare earth permanent-magnetic material with highest magnetic energy product, theoretical magnetic energy
Product may be up to 64MGOe, there is the title of " magnetic king ".As instantly most widely used rare earth permanent-magnetic material, Nd-Fe-B base permanent magnetism
Material is also the commercialization magnetic material that cost performance is optimal so far.A few days ago, Chinese Nd-Fe-B based permanent magnetic material industry has been
Nearly the 80% of world market total amount is accounted for, is the industry center of global Nd-Fe-B based permanent magnetic material.But due to being sintered neodymium iron
B permanent magnetic material is a kind of powdered metallurgical material that chemical activity is strong, and magnet surface is easy the oxidation that is corroded, greatly limits
The application of Neodymium iron boron magnetic product in the industrial production.Currently, most often being taken to improve the corrosion resistance of neodymium iron boron magnetic body
Method mainly has alloying and surface addition protective layer method, and still, often the former is usually to sacrifice magnet magnetic property as cost,
And effect is unobvious, therefore, the method for surface addition protective layer method becomes current neodymium iron boron industry and improves magnet corrosion resisting property
Main means.
Currently, aluminium protective layer is the technique of optimal development prospect in neodymium iron boron surfacecti proteon field.The knot of aluminium protective layer
With joint efforts and corrosion resistance is above the metal protection layers such as general nickel protective layer and zinc protective layer.But aluminium protective layer also has
The defect of its own, it is low that there is surface hardnesses, easily scratches and corrosion resistance still needs the problems such as being further increased urgently
It solves.
Summary of the invention
In view of the above-mentioned problems, it is an object of the invention to: it is multiple to provide a kind of original position for neodymium iron boron magnetic body surfacecti proteon
Coating and preparation method thereof is closed, so that magnet surface, which obtains, has high-compactness, highly corrosion resistant, higher hardness and higher resistance to
Aluminium/aluminium oxide In-situ reaction coating of the advantages such as mill property；And fitness, binding force and the stability of In-situ reaction coating also superior to
Simple Double-layer aluminum-alumina composite coating.
To achieve the goals above, the technical scheme adopted by the invention is as follows:
A kind of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon, the In-situ reaction coating include that fine aluminium applies
Layer and aluminum oxide film；The top of pure aluminum coating is arranged in the aluminum oxide film, wherein pure aluminum coating is with a thickness of 100-
600 microns, aluminum oxide film with a thickness of 6-30 microns.
A kind of preparation method of the In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon, the specific steps are as follows:
S1: the pre-treatment of neodymium iron boron magnetic body:
Remove the impurity and oxide on neodymium iron boron magnetic body surface；
S2: the preparation of spray coating liquor
It is 28-32s as spray coating liquor that fine aluminium solution, which is diluted to viscosity,；
S3: the spraying and solidification of neodymium iron boron magnetic body surface pure aluminum coating:
Neodymium iron boron magnetic body after pre-treatment is placed in spraying working platform, is passing through neodymium iron boron magnetic body using high speed stream of nitrogen gas
Surface sprays pure aluminum coating, carries out curing process after spraying；
S4: the removing surface of pure aluminum coating:
Degreasing, neutralization and washing process are carried out to the neodymium iron boron magnetic body surface after spraying pure aluminum coating；
S5: anodic oxidation process:
By step S4, treated that neodymium iron boron magnetic body is quickly placed into oxalic acid carries out anodized, in fine aluminium
One layer of aluminum oxide film of coating surface in-situ preparation；
S6: the high temperature closure processing of aluminum oxide film:
Neodymium iron boron magnetic body after anodic oxidation is placed in progress high temperature closure processing in nickel acetate solution.
Preferably, detailed process is as follows by step S1: by neodymium iron boron magnetic body by removing in chamfering, alkaline thermal debinding degreasing fluid
Oil, the dry and progress 25-35s pickling in the 65% of 50-60ml/L nitric acid solution, remove the miscellaneous of neodymium iron boron magnetic body surface
Matter and oxide, are finally cleaned by ultrasonic 1-3min in deionized water.
Preferably, detailed process is as follows by step S2: fine aluminium solution is placed in pneumatic stirring platform, first opens nitrogen valve,
Then pneumatic stirring knob is opened, starts to stir, mixing time 30-40min；Fine aluminium solution and dilution after stirring press body
Product obtains the spray coating liquor that viscosity is 28-32s than 4-6:1 after mixing.
Preferably, it is as follows that actual conditions are sprayed in step S3: spray distance 25-35mm, nitrogen gas pressure 0.2-
0.4MPa, spraying rate 15-20cm/s, adjust flow knob, and flow control is slightly wet in each spraying end workpiece surface
Profit is advisable, and after the pure aluminum coating that preparation is evenly distributed on neodymium iron boron magnetic body surface, carries out 115-125 DEG C of precuring and 225-235
DEG C curing process.
Preferably, step S4's is specific as follows: it is 50-70 DEG C that sample, which is placed in temperature, first, and concentration is 80-120g/L's
Degreasing in 1-3 minutes is carried out in hot sodium hydroxide solution；Then, sample is placed in the nitric acid solution that concentration is 300-400g/L and is soaked
Neutralization is washed, embathing the time is 3-5 minutes；Finally, and then being cleaned with hot water with after cold water wash, wherein when hot water cleans
Temperature is 40-60 DEG C.
Preferably, the design parameter of step S5 Anodic Oxidation is provided that electrolyte concentration of oxalic acid is 5-10%, electric current
Density is DC0.5-1A/dm2, voltage 25-30V, temperature is 20-29 DEG C, anodizing time 20-60min.
Preferably, the specific method is as follows for step S6 high temperature Seal treatment: by 1.4-1.8g/LNi2+Ion, quality point
Number is the acetic acid of 0.4-0.8%, and configuration pH value is 5-7's after the organic additive mixing that mass fraction is 0.01-0.03%
Mixed solution, by step S5, treated that neodymium iron boron magnetic body is placed in above-mentioned mixed solution, in 82-98 DEG C, reacts 10-20min.
Preferably, the organic additive is high temperature hole sealing agent DY103.
The beneficial effects of the present invention are:
In-situ composite aluminum/aluminum oxide coating layer of the present invention has high-compactness, highly corrosion resistant, high rigidity and high-wearing feature
Etc. advantages aluminium/aluminium oxide In-situ reaction coating；And fitness, binding force and the stability of In-situ reaction coating are also superior to simple
Double-layer aluminum-alumina composite coating.
Detailed description of the invention
Fig. 1 is neodymium iron boron magnetic body surface in situ composite coating schematic diagram；
1- aluminum oxide film, 2- pure aluminum coating, 3- neodymium iron boron magnetic body in appended drawing reference.
Specific embodiment
The present invention is further illustrated with reference to embodiments, it should be noted that is only to present inventive concept
Example and explanation, affiliated those skilled in the art make various modifications to described specific embodiment
Or supplement or be substituted in a similar manner, as long as it does not deviate from the concept of invention or surmount model defined in the claims
It encloses, is regarded as falling into protection scope of the present invention.
Embodiment 1
A kind of In-situ reaction coating and preparation method thereof for neodymium iron boron magnetic body surfacecti proteon, comprising the following steps:
S1: the pre-treatment of neodymium iron boron magnetic body:
The blocky neodymium iron boron magnetic body for being 40 millimeters × 20 millimeters × 15 millimeters with specification is (by Anhui the earth bear new material share
Co., Ltd provides, the trade mark: 48H) it is tested, by neodymium iron boron magnetic body by oil removing in chamfering, alkaline thermal debinding degreasing fluid, dry
The dry and progress 30s pickling in the 65% of 55ml/L nitric acid solution, removes the impurity and oxide on neodymium iron boron magnetic body surface,
Finally it is cleaned by ultrasonic 2min in deionized water.
S2: the preparation of spray coating liquor
Fine aluminium solution is placed in pneumatic stirring platform, first opens nitrogen valve, pneumatic stirring knob is then opened, starts to stir
It mixes, mixing time 35min；(become rusty diluent SL for the model Tyke of dilution, is purchased from for fine aluminium solution and dilution after stirring
Atotech) by volume 5:1 obtain after mixing viscosity be 30s spray coating liquor.
S3: the spraying and solidification of neodymium iron boron magnetic body surface pure aluminum coating:
Neodymium iron boron magnetic body after pre-treatment is placed in spraying working platform, is passing through neodymium iron boron magnetic body using high speed stream of nitrogen gas
Surface sprays pure aluminum coating, carries out curing process after spraying；Spraying actual conditions are: spray distance 25mm, nitrogen gas pressure
0.3MPa, spraying rate 18cm/s adjust flow knob, and flow control moistens slightly in each spraying end workpiece surface is
Preferably.After the pure aluminum coating that preparation is evenly distributed on neodymium iron boron magnetic body surface, 120 DEG C of precuring and 230 DEG C of curing process are carried out.
S4: the removing surface of pure aluminum coating:
It is 60 DEG C that sample, which is placed in temperature, first, carries out degreasing in 2 minutes in the hot sodium hydroxide solution that concentration is 100g/L；
Then, sample is placed in the nitric acid solution that concentration is 350g/L and embathes neutralization, embathing the time is 4 minutes；Finally, clear with cold water
It is and then cleaned with hot water after washing, wherein temperature when hot water cleans is 50 DEG C.
S5: anodic oxidation process:
By step S4, treated that neodymium iron boron magnetic body is quickly placed into oxalic acid carries out anodized, in fine aluminium
One layer of aluminum oxide film of coating surface in-situ preparation；The design parameter of anodic oxidation is provided that electrolyte concentration of oxalic acid is
8%, current density DC0.8A/dm2, voltage 28V, temperature is 25 DEG C, anodizing time 40min.
S6: the high temperature closure processing of aluminum oxide film:
Neodymium iron boron magnetic body after anodic oxidation is placed in progress high temperature closure processing in nickel acetate solution, high temperature closure processing
The specific method is as follows: by 1.6g/LNi2+Ion, the acetic acid that mass fraction is 0.5%, the high temperature that mass fraction is 0.02% seal
The mixed solution that configuration pH value is 6 after hole agent DY103 mixing, by step S5, treated that neodymium iron boron magnetic body is placed in above-mentioned mixing
In solution, in 92 DEG C, 15min is reacted.
Embodiment 2
The preparation method is the same as that of Example 1 for the present embodiment, the difference is that spray gun distance is 30mm in step S3.
Embodiment 3
The preparation method is the same as that of Example 1 for the present embodiment, the difference is that spray gun distance is 35mm in step S3.
Embodiment 4
The preparation method of the present embodiment is with embodiment 2, the difference is that step S5 mesoxalic acid concentration of electrolyte is 10%.
Embodiment 5
The preparation method of the present embodiment is with embodiment 2, the difference is that current density is DC1A/dm in step S52。
Embodiment 6
The preparation method of the present embodiment is with embodiment 5, the difference is that voltage is 30V in step S5.
Embodiment 7
The preparation method of the present embodiment is with embodiment 6, the difference is that the step S5 Anodic Oxidation time is 20min.
Embodiment 8
Embodiment 8: the preparation method of the present embodiment with embodiment 6, unlike the step S5 Anodic Oxidation time be
45min。
Embodiment 9
The preparation method of the present embodiment is with embodiment 6, the difference is that the step S5 Anodic Oxidation time is 60min.
Test example
Carrying out salt fog and micro-hardness testing test, concrete outcome to the product of specific embodiment 1-9 preparation see the table below:
| Product (embodiment) | Salt spray test (hour) | Microhardness (HV) |
| Specific embodiment 1 | 176 | 379 |
| Specific embodiment 2 | 188 | 398 |
| Specific embodiment 3 | 182 | 385 |
| Specific embodiment 4 | 180 | 383 |
| Specific embodiment 5 | 181 | 386 |
| Specific embodiment 6 | 178 | 381 |
| Specific embodiment 7 | 179 | 382 |
| Specific embodiment 8 | 183 | 390 |
| Specific embodiment 9 | 182 | 386 |
Through the foregoing embodiment it can be found that in-situ composite aluminum/aluminum oxide coating layer of the present invention is resistance to high-compactness, height
The aluminium of the advantages such as corrosivity, higher hardness and higher abrasion resistance/aluminium oxide In-situ reaction coating.
Claims (9)
1. a kind of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon, it is characterised in that: the In-situ reaction coating
Including pure aluminum coating and aluminum oxide film；The top of pure aluminum coating is arranged in the aluminum oxide film, wherein pure aluminum coating is thick
Degree be 100-600 microns, aluminum oxide film with a thickness of 6-30 microns.
2. a kind of preparation method of the In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon, it is characterised in that: specific steps
It is as follows:
S1: the pre-treatment of neodymium iron boron magnetic body:
Remove the impurity and oxide on neodymium iron boron magnetic body surface；
S2: the preparation of spray coating liquor
It is 28-32s as spray coating liquor that fine aluminium solution, which is diluted to viscosity,；
S3: the spraying and solidification of neodymium iron boron magnetic body surface pure aluminum coating:
Neodymium iron boron magnetic body after pre-treatment is placed in spraying working platform, is passing through neodymium iron boron magnetic body surface using high speed stream of nitrogen gas
Pure aluminum coating is sprayed, carries out curing process after spraying；
S4: the removing surface of pure aluminum coating:
Degreasing, neutralization and washing process are carried out to the neodymium iron boron magnetic body surface after spraying pure aluminum coating；
S5: anodic oxidation process:
By step S4, treated that neodymium iron boron magnetic body is quickly placed into oxalic acid carries out anodized, in pure aluminum coating
Surface in situ generates one layer of aluminum oxide film；
S6: the high temperature closure processing of aluminum oxide film:
Neodymium iron boron magnetic body after anodic oxidation is placed in progress high temperature closure processing in nickel acetate solution.
3. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 2,
It is characterized by: detailed process is as follows by step S1: by neodymium iron boron magnetic body by oil removing in chamfering, alkaline thermal debinding degreasing fluid,
The dry and progress 25-35s pickling in the 65% of 50-60ml/L nitric acid solution, removes the impurity on neodymium iron boron magnetic body surface
And oxide, finally it is cleaned by ultrasonic 1-3min in deionized water.
4. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 2,
It is characterized by: detailed process is as follows by step S2: fine aluminium solution being placed in pneumatic stirring platform, first opens nitrogen valve, then
Pneumatic stirring knob is opened, starts to stir, mixing time 30-40min；Fine aluminium solution and dilution after stirring are by volume
4-6:1 obtains the spray coating liquor that viscosity is 28-32s after mixing.
5. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 2,
It is characterized by: it is as follows to spray actual conditions in step S3: spray distance 25-35mm, nitrogen gas pressure 0.2-0.4MPa, spray
Painting speed is 15-20cm/s, adjusts flow knob, and flow control moistens slightly in each spraying end workpiece surface to be advisable,
After the pure aluminum coating that the preparation of neodymium iron boron magnetic body surface is evenly distributed, carry out at 115-125 DEG C of precuring and 225-235 DEG C of solidification
Reason.
6. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 2,
It is characterized by: step S4's is specific as follows: it is 50-70 DEG C that sample, which is placed in temperature, first, and concentration is the hot hydrogen of 80-120g/L
Degreasing in 1-3 minutes is carried out in sodium hydroxide solution；Then, sample is placed in the nitric acid solution that concentration is 300-400g/L in embathing
With, embathe the time be 3-5 minutes；Finally, and then being cleaned with hot water with after cold water wash, wherein temperature when hot water cleans
It is 40-60 DEG C.
7. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 2,
It is characterized by: the design parameter of step S5 Anodic Oxidation is provided that electrolyte concentration of oxalic acid is 5-10%, current density
For DC0.5-1A/dm2, voltage 25-30V, temperature is 20-29 DEG C, anodizing time 20-60min.
8. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 2,
It is characterized by: the specific method is as follows for step S6 high temperature Seal treatment: by 1.4-1.8g/LNi2+Ion, mass fraction are
The acetic acid of 0.4-0.8%, the mixing that configuration pH value is 5-7 after the organic additive mixing that mass fraction is 0.01-0.03%
Solution, by step S5, treated that neodymium iron boron magnetic body is placed in above-mentioned mixed solution, in 82-98 DEG C, reacts 10-20min.
9. a kind of preparation method of In-situ reaction coating for neodymium iron boron magnetic body surfacecti proteon according to claim 8,
It is characterized by: the organic additive is high temperature hole sealing agent DY103.
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| CN110129733A (en) * | 2019-06-19 | 2019-08-16 | 东北大学 | A kind of Sintered NdFeB magnet and preparation method thereof with composite film |
| CN110828099A (en) * | 2019-11-21 | 2020-02-21 | 内蒙古工业大学 | Neodymium-iron-boron magnet surface composite corrosion-resistant coating and preparation method thereof |
| CN117542599A (en) * | 2023-10-23 | 2024-02-09 | 江苏普隆磁电有限公司 | Corrosion-resistant NdFeB magnet and preparation method thereof |
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| CN110129733A (en) * | 2019-06-19 | 2019-08-16 | 东北大学 | A kind of Sintered NdFeB magnet and preparation method thereof with composite film |
| CN110828099A (en) * | 2019-11-21 | 2020-02-21 | 内蒙古工业大学 | Neodymium-iron-boron magnet surface composite corrosion-resistant coating and preparation method thereof |
| CN117542599A (en) * | 2023-10-23 | 2024-02-09 | 江苏普隆磁电有限公司 | Corrosion-resistant NdFeB magnet and preparation method thereof |
| CN117542599B (en) * | 2023-10-23 | 2024-06-14 | 江苏普隆磁电有限公司 | Corrosion-resistant NdFeB magnet and preparation method thereof |
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