CN107419231B - The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating and Nd-Fe-B permanent magnet with the coating - Google Patents
The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating and Nd-Fe-B permanent magnet with the coating Download PDFInfo
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- CN107419231B CN107419231B CN201710616213.0A CN201710616213A CN107419231B CN 107419231 B CN107419231 B CN 107419231B CN 201710616213 A CN201710616213 A CN 201710616213A CN 107419231 B CN107419231 B CN 107419231B
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 165
- 239000011248 coating agent Substances 0.000 title claims abstract description 70
- 238000000576 coating method Methods 0.000 title claims abstract description 70
- 238000005260 corrosion Methods 0.000 title claims abstract description 52
- 238000009413 insulation Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 230000004913 activation Effects 0.000 claims abstract description 59
- 239000011241 protective layer Substances 0.000 claims abstract description 59
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 50
- 239000011230 binding agent Substances 0.000 claims abstract description 36
- 238000000151 deposition Methods 0.000 claims abstract description 34
- 238000004544 sputter deposition Methods 0.000 claims abstract description 34
- 230000007704 transition Effects 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000011265 semifinished product Substances 0.000 claims abstract description 23
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 6
- 231100000719 pollutant Toxicity 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 61
- 238000004140 cleaning Methods 0.000 claims description 56
- 150000002500 ions Chemical class 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 28
- 239000010410 layer Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 21
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229910052718 tin Inorganic materials 0.000 claims description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000292 calcium oxide Substances 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- 229910020994 Sn-Zn Inorganic materials 0.000 claims description 9
- 229910009069 Sn—Zn Inorganic materials 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910002796 Si–Al Inorganic materials 0.000 claims description 8
- 229910007570 Zn-Al Inorganic materials 0.000 claims description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 20
- 230000004907 flux Effects 0.000 abstract description 19
- 150000003839 salts Chemical class 0.000 description 33
- 239000007921 spray Substances 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 26
- 238000012360 testing method Methods 0.000 description 24
- 238000000034 method Methods 0.000 description 20
- 230000008021 deposition Effects 0.000 description 19
- 230000007797 corrosion Effects 0.000 description 18
- 238000007747 plating Methods 0.000 description 13
- 239000011135 tin Substances 0.000 description 9
- 239000011701 zinc Substances 0.000 description 8
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000010949 copper Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910017083 AlN Inorganic materials 0.000 description 3
- 238000001962 electrophoresis Methods 0.000 description 3
- 229920006334 epoxy coating Polymers 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910000570 Cupronickel Inorganic materials 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910019912 CrN Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PXAWCNYZAWMWIC-UHFFFAOYSA-N [Fe].[Nd] Chemical compound [Fe].[Nd] PXAWCNYZAWMWIC-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- OPXJEFFTWKGCMW-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Ni].[Cu] OPXJEFFTWKGCMW-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The present invention proposes a kind of preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating and the Nd-Fe-B permanent magnet with the coating, fastness and the good Nd-Fe-B permanent magnetic anti-corrosion insulation coating of anticorrosion effect can be prepared under the premise of not influencing Nd-Fe-B permanent magnet magnetic flux.The preparation method includes the following steps: to clean semi-finished product surface of Nd-Fe-B permanent magnet, dry after removing pollutant；The Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, is activated using surface of the ion source to the Nd-Fe-B permanent magnet；The vacuum coating area that Nd-Fe-B permanent magnet after activation is moved to vacuum coating equipment is sequentially depositing binder course, inner protective layer, transition zone and external protection using the surface of the Nd-Fe-B permanent magnet of vacuum magnetic-control sputtering mode after activation at≤100 DEG C.
Description
Technical field
The invention belongs to the technical field of surface of Nd-Fe-B permanent magnet material more particularly to a kind of Nd-Fe-B permanent magnetic anti-corrosions
The preparation method of insulating blanket and Nd-Fe-B permanent magnet with the coating.
Background technique
Nd-Fe-B permanent magnet material (chemical name NdFeB) belongs to third generation rare earth permanent magnet, because have high remanent magnetism, high-coercive force and
The characteristics such as high energy product are widely used in New-energy electric vehicle, magneto used for wind power generation, magnetic suspension, unmanned plane etc.
Numerous southern exposure industries.Although Nd-Fe-B permanent magnet material has excellent magnetic property, corrosion resistance is poor, thus, existing
Have in technology, usually plate protective layer in neodymium-iron-boron permanent magnetic material surface, leads to the reduction of its magnetic property to avoid because of magnet corrosion,
It prolongs its service life.
Currently, traditional method is wet using plating or chemical plating etc. there are many anti-corrosion methods of Nd-Fe-B permanent magnet material
Method technique uses this wet processing in surface of Nd-Fe-B permanent magnet plated with nickel, zinc or nickel-copper-nickel composite layer, once plating
Liquid penetrates into the internal void of Nd-Fe-B permanent magnet, will cause the accelerated corrosion of permanent magnet instead.With surface coating technology
Development has the method using dry process such as Vacuum Depositions in neodymium-iron-boron permanent magnetic material surface plating protective layer in the prior art,
Overcome the deficiency of wet processing.Such as: it is vacuum aluminum-coated that patent CN101736304A discloses a kind of surface of Nd-Fe-B permanent magnet
Method uses the method for magnetic control multi arc sputtering to plate complete and corrosion resistant aluminium coat in surface of Nd-Fe-B permanent magnet.However,
There are still some shortcomings for this method: (1) it is vacuum aluminum-coated to be completed at a high temperature of 250 DEG C -300 DEG C, although improving coating
Salt spray resistance ability, but can have the potential risk that Nd-Fe-B permanent magnet magnetic flux reduces through high-temperature process；(2) existing method is logical
Single layer aluminium film only often is plated on the surface of Nd-Fe-B permanent magnet, is bound directly between coating and Nd-Fe-B permanent magnet, pinning effect
On the weak side, the fastness and anticorrosion effect of coating can decrease.
Therefore, how under the premise of not influencing Nd-Fe-B permanent magnet magnetic flux, fastness and anticorrosion effect are prepared more
Good Nd-Fe-B permanent magnetic anti-corrosion insulation coating is a current technical problem urgently to be solved.
Summary of the invention
The present invention for the above technical issues, proposes the preparation method and tool of a kind of Nd-Fe-B permanent magnetic anti-corrosion insulation coating
There is the Nd-Fe-B permanent magnet of the coating, this method can prepare under the premise of not influencing Nd-Fe-B permanent magnet magnetic flux
Fastness and the good Nd-Fe-B permanent magnetic anti-corrosion insulation coating of anticorrosion effect.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
The present invention proposes a kind of preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating, includes the following steps:
Surface preparation: cleaning semi-finished product surface of Nd-Fe-B permanent magnet is dried after removing pollutant；
Surface active: the Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, using ion source pair
The surface of the Nd-Fe-B permanent magnet is activated；
Vacuum coating: the Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, at≤100 DEG C
Under, binder course, inner protective layer, mistake are sequentially depositing using the surface of the Nd-Fe-B permanent magnet of vacuum magnetic-control sputtering mode after activation
Cross layer and external protection.
Preferably, the binder course with a thickness of 10nm-1000nm, the inner protective layer with a thickness of 1 μm -10 μm,
The transition zone with a thickness of 10nm-1000nm, the external protection with a thickness of 0.3 μm -6 μm.
Preferably, the material of the binder course is selected from one of Al, Cr, Ti or stainless steel or a variety of.
Preferably, the material of the inner protective layer is selected from one of Sn, Zn, Cu, Al, Si-Al, Zn-Al or Sn-Zn
Or it is a variety of.
Preferably, the material of the transition zone is selected from Sn, Zn, Al, Si-Al, Zn-Al, Sn-Zn, SnO2, ZnO or
Al2O3One of or it is a variety of.
Preferably, the material of the external protection is selected from Al2O3、AlN、Cr2O3、TiO2、SiO2、Si3N4, TiN or CrN
One of or it is a variety of.
Preferably, cleaning the specific steps of semi-finished product surface of Nd-Fe-B permanent magnet in the surface pre-treatment step
It include: that semi-finished product Nd-Fe-B permanent magnet is placed in cleaning solution to clean；It takes out after cleaning, is rinsed using deionized water；Drift
It is taken out after washing, is placed in supersonic cleaning machine and is cleaned by ultrasonic；It is taken out after ultrasonic cleaning, secondary rinsing is carried out using deionized water.
Preferably, the composition of the cleaning solution are as follows: sodium carbonate 5g/L-10g/L, anhydrous calcium oxide 15g/L-20g/L, hydrogen
Sodium oxide molybdena 10g/L-40g/L, solvent are water；The ultrasonic cleaning time is 0.5min-5min.
Preferably, the vacuum degree in the ion activation area is 0.05Pa-3Pa, described in the activation step
The power of ion source is 3kW-7kW, activation time 0.5min-3min.
The present invention also provides the Nd-Fe-B permanent magnet that a kind of surface has anti-corrosion insulation coating, the anti-corrosion insulation coating
It is prepared using the preparation method as described in any of the above-described technical solution.
Compared with prior art, the advantages and positive effects of the present invention are:
1, the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention utilizes vacuum at≤100 DEG C
The coating of surface of Nd-Fe-B permanent magnet deposition multilayered structure of the magnetron sputtering mode after ion source activation, the coating of acquisition have
Good Corrosion Protection；
2, the coating prepared using the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention, is being had
While having good Corrosion Protection, Nd-Fe-B permanent magnet magnetic flux is not influenced, while also there is insulation characterisitic, can satisfy
Multiple functions requirement of the various magneto fields to Nd-Fe-B permanent magnet coating, the scope of application are more extensive.
Detailed description of the invention
Fig. 1 is the structural representation for the Nd-Fe-B permanent magnet that surface provided by the embodiment of the present invention has anti-corrosion insulation coating
Figure；
In figure, 1, external protection；2, transition zone；3, inner protective layer；4, binder course；5, semi-finished product Nd-Fe-B permanent magnet.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The embodiment of the invention provides a kind of preparation methods of Nd-Fe-B permanent magnetic anti-corrosion insulation coating, include the following steps:
S1 surface preparation: cleaning semi-finished product surface of Nd-Fe-B permanent magnet is dried after removing pollutant.
In this step, by the pollutant of cleaning removal surface of Nd-Fe-B permanent magnet, especially grease etc., after being conducive to
It is continuous to carry out plated film.It should be noted that being completely standard by surface contaminant removal when cleaning.
Further, this step is dried after cleaning, can be removed the moisture inside Nd-Fe-B permanent magnet, be avoided shadow
Ring anti-corrosion effect.It should be noted that select drying temperature to be advisable for 50 DEG C -120 DEG C in drying, and such as: drying temperature can
Think 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C etc., this is because: drying temperature is lower than 50 DEG C,
Drying effect is poor, has moisture and penetrates into inside Nd-Fe-B permanent magnet, influences anti-corrosion effect；And drying temperature is higher than 120 DEG C, deposits
In the potential risk for influencing Nd-Fe-B permanent magnet magnetic property.Drying time selection 2min-7min is advisable, for example, drying time can
Think 2min, 3min, 4min, 5min, 6min, 7min etc., that is, can guarantee that Nd-Fe-B permanent magnet is sufficiently dried, and can avoid drying
Overlong time causes to waste.It is understood that those skilled in the art can according to after cleaning Nd-Fe-B permanent magnet it is wet
Situation specifically adjusts drying condition, for example, drying time can suitably shorten when the drying temperature of selection is slightly higher；The drying of selection
When temperature is slightly lower, drying time can be appropriately extended.
In addition it is also necessary to which explanation, semi-finished product Nd-Fe-B permanent magnet described in this step refer to that machining finishes
By the Nd-Fe-B permanent magnet of chamfer polishing, finished product neodymium can be directly obtained after this semi-finished product surface of Nd-Fe-B permanent magnet plated film
Iron boron permanent magnet.
S2 surface active: the Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, using ion source
The surface of the Nd-Fe-B permanent magnet is activated.
In this step, it is activated using surface of the ion source to Nd-Fe-B permanent magnet, neodymium iron boron can be made forever
The arrow of magnet surface can improve 1 magnitude, reduce subsequent plating layer energy barrier required in conjunction with surface of Nd-Fe-B permanent magnet, favorably
In the combination of subsequent plating layer, the fastness of coating is improved.
S3 vacuum coating: the Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, at≤100 DEG C
Under, binder course, inner protective layer, mistake are sequentially depositing using the surface of the Nd-Fe-B permanent magnet of vacuum magnetic-control sputtering mode after activation
Cross layer and external protection.
In this step, it should be noted that vacuum coating is carried out at≤100 DEG C, it is normal compared to vacuum magnetic-control sputtering
200 DEG C or more of the high-temperature process used, can be avoided influence of the high-temperature process to Nd-Fe-B permanent magnet magnetic flux；Moreover, this
In embodiment, surface of Nd-Fe-B permanent magnet plates binder course first by being activated to enhance coating and neodymium iron when plated film
The combination of boron permanent magnet surfaces, thus, even if carrying out vacuum coating at≤100 DEG C, it still is able to guarantee the jail that coating combines
Solidity.It is understood that those skilled in the art can be according to the specific material and thickness requirement of coating, it is suitable to be specifically chosen
Temperature, such as: temperature when vacuum coating can be 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C etc..In addition,
Regulated and controled it should also be noted that, the cooling mode of water can be used in sputter temperature when vacuum coating.
Further, the coating in this step includes binder course, inner protective layer, transition zone and external protection, wherein in conjunction with
Layer primarily serves the effect for improving inner protective layer adhesive force, and the material of binder course should be with Nd-Fe-B permanent magnet material and interior protection
Layer material has stronger compatibility；Inner protective layer can play the role of blocking Nd-Fe-B permanent magnet internal flaw；Transition zone master
Play the role of connecting inner protective layer and external protection, the material of transition zone should be with inner protective layer material and external protection material
Material has stronger compatibility；External protection primarily serves insulation, erosion-resisting effect.Compared to existing single plating layer, this step
The combination of the coating and surface of Nd-Fe-B permanent magnet of this multilayered structure used in rapid is stronger, and uses inner protective layer
With two layers of protective layer of external protection, anticorrosion effect is more preferable.
In addition it is also necessary to explanation, apart from the temperature, the other conditions and existing vacuum magnetic control that vacuum magnetic-control sputtering uses
Sputtering condition is similar, such as: the vacuum degree in vacuum coating area is 0.05Pa-1Pa, sputtering power 15kW-40kW, it is possible to understand that
, those skilled in the art can be specifically chosen and suitable vacuum degree and splash according to the specific material and thickness requirement of coating
Power is penetrated, such as: vacuum degree can be 0.05Pa, 0.1Pa, 0.3Pa, 0.5Pa, 0.8Pa, 1Pa etc., and sputtering power can be
15kW, 20kW, 25kW, 30kW, 40kW etc..When vacuum coating, since binder course, inner protective layer, transition zone and external protection are adopted
Material may be different, thus, it can be deposited respectively in the different zones in vacuum coating area, different splash can be used in different zones
Penetrate temperature, vacuum degree and sputtering power.
The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention utilizes Vacuum Magnetic at≤100 DEG C
The coating of surface of Nd-Fe-B permanent magnet deposition multilayered structure of the sputtering mode after ion source activation is controlled, the coating of acquisition has good
Good Corrosion Protection.Moreover, being prepared using the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention
Coating do not influence Nd-Fe-B permanent magnet magnetic flux while with good Corrosion Protection, while also having insulation special
Property, it can satisfy multiple functions requirement of the various magneto fields to Nd-Fe-B permanent magnet coating, the scope of application is more extensive.
In a preferred embodiment, the binder course with a thickness of 10nm-1000nm, the inner protective layer with a thickness of 1 μ
M-10 μm, the transition zone with a thickness of 10nm-1000nm, the external protection with a thickness of 0.3 μm -6 μm.It is preferred real at this
It applies in example, further defines the thickness of binder course, inner protective layer, transition zone and external protection, which is optimal model
It encloses, wherein the thickness of binder course and transition zone mainly influences the fastness of coating, and the thickness of inner protective layer and external protection is main
The corrosion resistance for influencing coating, only when the thickness of binder course, inner protective layer, transition zone and external protection is mutually matched,
The coating that not only there is good corrosion resistance but also be firmly combined can be obtained.It is understood that those skilled in the art can basis
The requirement for anticorrosion of coating is specifically chosen the thickness of each layer, such as: the thickness of binder course can for 10nm, 50nm, 100nm,
300nm, 500nm, 700nm, 1000nm etc., the thickness of inner protective layer can be 1 μm, 3 μm, 5 μm, 7 μm, 9 μm, 10 μm etc., mistake
The thickness for crossing layer can be for 10nm, 50nm, 100nm, 300nm, 500nm, 700nm, 1000nm etc., and the thickness of external protection can be with
It is 0.3 μm, 0.5 μm, 1 μm, 2 μm, 4 μm, 6 μm etc..
In a preferred embodiment, the material of the binder course is selected from one of Al, Cr, Ti or stainless steel or a variety of.
In the preferred embodiment, the material of binder course is further defined, these materials and Nd-Fe-B permanent magnet have stronger parent
And property, be conducive to the fastness for improving coating.It is understood that those skilled in the art can be according to the material of inner protective layer
Selection suitably combines layer material.
In a preferred embodiment, the material of the inner protective layer is selected from Sn, Zn, Cu, Al, Si-Al, Zn-Al or Sn-Zn
One of or it is a variety of.In the preferred embodiment, the material of inner protective layer is further defined, these materials have stronger
Corrosion resistance and the performance for blocking magnet surface hole are conducive to the corrosion resistance for improving coating.It is understood that ability
Field technique personnel can select suitable inner protective layer material according to the application environment of Nd-Fe-B permanent magnet and requirement for anticorrosion.
In a preferred embodiment, the material of the transition zone is selected from Sn, Zn, Al, Si-Al, Zn-Al, Sn-Zn, SnO2、
ZnO or Al2O3One of or it is a variety of.In the preferred embodiment, further define the material of transition zone, these materials with
Resistant material as inner protective layer and external protection has stronger compatibility, is conducive to improve inner protective layer and outer protection
The connectivity robustness of layer.It is understood that those skilled in the art can select according to the material of inner protective layer and external protection
Select suitable buffer layer material.
In a preferred embodiment, the material of the external protection is selected from Al2O3、AlN、Cr2O3、TiO2、SiO2、Si3N4、
One of TiN or CrN or a variety of.In the preferred embodiment, the material of external protection is further defined, these materials tool
There are stronger corrosion resistance and insulation performance, is conducive to the corrosion resistance and insulating properties that improve coating.It is understood that this
Field technical staff can require to select suitable external protection material according to the application environment and anti-corrosion insulation of Nd-Fe-B permanent magnet
Material.
In a preferred embodiment, in the surface pre-treatment step, cleaning semi-finished product surface of Nd-Fe-B permanent magnet
Specific steps include: that semi-finished product Nd-Fe-B permanent magnet is placed in cleaning solution to clean；It is taken out after cleaning, using deionized water
Rinsing；It is taken out after rinsing, is placed in supersonic cleaning machine and is cleaned by ultrasonic；It takes out, is carried out using deionized water secondary after ultrasonic cleaning
Rinsing.In the preferred embodiment, the specific steps of cleaning semi-finished product surface of Nd-Fe-B permanent magnet are further defined, by clear
Washing lotion cleaning is cleaned by ultrasonic and rinses twice, can guarantee the pollutant removal of surface of Nd-Fe-B permanent magnet is clean.
In further preferred embodiments, the composition of the cleaning solution are as follows: sodium carbonate 5g/L-10g/L, anhydrous calcium oxide
15g/L-20g/L, sodium hydroxide 10g/L-40g/L, solvent are water；The ultrasonic cleaning time is 0.5min-5min.It is excellent at this
It selects in embodiment, further defines the composition of cleaning solution and the time of ultrasonic cleaning, the composition of the cleaning solution and ultrasonic cleaning
Time is optimized scope, will cause certain adverse effect when exceeding this range.Such as: it is formed for cleaning solution, when each
When the concentration of component is lower than the lower limit of optimized scope, it is understood that there may be clean sordid phenomenon, and then influence the anti-corrosion effect of coating
Fruit；When the concentration of each component is higher than the upper limit of optimized scope, in fact it could happen that cross and wash phenomenon, caused to surface of Nd-Fe-B permanent magnet
Slight erosion influences coating anti-corrosion effect.It is understood that those skilled in the art can be according to surface of Nd-Fe-B permanent magnet
Pollution level, be specifically chosen suitable cleaning solution composition, such as: the concentration of sodium carbonate can be 5g/L, 7.5g/L, 10g/L
Concentration Deng, anhydrous calcium oxide can be 15g/L, 17.5g/L, 20g/L etc., and the concentration of sodium hydroxide can be 10g/L, 20g/
L, 30g/L, 40g/L etc..For the ultrasonic cleaning time, when being cleaned by ultrasonic the time lower than 0.5 minute, cleaning effect may not
Obviously, when being cleaned by ultrasonic the time higher than 5 minutes, cleaning quality will not obtain more Gao Tisheng, will cause the energy instead
Waste.It is understood that those skilled in the art can be specifically chosen and close according to the pollution level of surface of Nd-Fe-B permanent magnet
The suitable ultrasonic cleaning time, such as: 0.5min, 1min, 3min, 5min etc..In addition, it should be noted that, except cleaning solution forms
Outside the ultrasonic cleaning time, in the process of cleaning, it is advisable in 1min-5min using the time that cleaning solution cleans, when rinsing adopts
It is advisable with the deionized water of 1 μ s/cm-10 μ s/cm, first time rinsing time is advisable in 1min-5min, and secondary rinsing time exists
It is advisable in 0.5min-3min, those skilled in the art can be specifically chosen as the case may be, to clean up, not occur to wash
Phenomenon and it is energy saving be standard.
In a preferred embodiment, in the activation step, the vacuum degree in the ion activation area is 0.05Pa-
3Pa, the power of the ion source are 3kW-7kW, activation time 0.5min-3min.In the preferred embodiment, it further limits
Determine surface active condition, which is optimal conditions, it will cause certain adverse effect when exceeding this range,
Only when activating vacuum degree, ion source power and activation time mutual cooperation, best surface-activation effect could be obtained.Example
Such as: being directed to vacuum degree, when vacuum degree is lower than 0.05Pa, ion source voltage potentially unstable influences surface-activation effect；Surely
When reciprocal of duty cycle is higher than 3Pa, the electric current of ion source is excessive, and stability may also reduce.For activation time, when activated between be lower than
When 0.5min, it is understood that there may be activate insufficient phenomenon；And activation can be guaranteed sufficiently by activating 3min, when continuing to extend activation
Between, activation effect will not be improved, leads to the waste of the energy afterwards instead.It is understood that those skilled in the art can root
According to coating material and requirement for anticorrosion, be specifically chosen suitable activation condition, such as: vacuum degree can for 0.05Pa, 0.1Pa,
0.5Pa, 1Pa, 2Pa, 3Pa etc., ion source power can for 3kW, 5kW, 7kW etc., activation time can for 0.5min, 1min,
2min, 3min etc..
As shown in Figure 1, another aspect of the present invention, which additionally provides a kind of surface, has the neodymium iron boron of anti-corrosion insulation coating forever
Magnet, the anti-corrosion insulation coating are prepared using preparation method described in any of the above-described embodiment.The Nd-Fe-B permanent magnetic
Body has good Corrosion Protection and insulation performance, and the remanent magnetism amount after magnetizing is higher, applied widely.
In order to become apparent from the preparation for introducing Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the embodiment of the present invention in detail
Method and Nd-Fe-B permanent magnet with the coating, are described below in conjunction with specific embodiment.
In whole embodiments, the semi-finished product Nd-Fe-B permanent magnet of use is after machining finishes through chamfer polishing
The trade mark is 45H, specification is 50mm × 23mm × 2.8mm semi-finished product Nd-Fe-B permanent magnet.In addition, to the Nd-Fe-B permanent magnetic of acquisition
Body has carried out salt spray test respectively, and tests the insulating properties and magnetic flux change of Nd-Fe-B permanent magnet before and after salt spray test respectively
To detect the destruction situation of coating.Wherein, salt spray test standard uses GB 6458-86 standard；Insulation performance test method are as follows:
The copper electrodes of conducting wire are had in the upper and lower surface covering of permanent magnet, contact two conducting wires, general-purpose simultaneously with two indicators of multimeter
The resistance value of table is the insulation numerical value of permanent magnet, and insulation numberical range is from infinity to zero；Magnetic flux is using Chinese metering section
Graduate HT707 intelligence fluxmeter is learned to be detected.
It is investigated respectively below for major parameter involved in each step and operating condition, and for example:
(1) influence that cleaning solution forms in surface pre-treatment step
Embodiment 1
S1 surface preparation: semi-finished product Nd-Fe-B permanent magnet being placed in cleaning solution and cleans 5min, the composition of cleaning solution are as follows:
Sodium carbonate 10g/L, anhydrous calcium oxide 20g/L, sodium hydroxide 40g/L, solvent are water；It is taken out after cleaning, using 10us/cm
Deionized water rinse 1min；It is taken out after rinsing, is placed in supersonic cleaning machine and is cleaned by ultrasonic 5min, the pH value of ultrasonic water is 6.5；
It is taken out after ultrasonic cleaning, secondary rinsing, rinsing time 1min is carried out using the deionized water of 10 μ s/cm；Taking-up is put into 80 DEG C
Drying box in dry 5min.
S2 surface active: the Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, ion activation area
Vacuum degree be 1Pa, use power to be activated for surface of the ion source of 3kW to Nd-Fe-B permanent magnet, activation time
For 3min.
S3 vacuum coating: the Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum degree
It is at 40 DEG C, using the Nd-Fe-B permanent magnetic of vacuum magnetic-control sputtering mode after activation for 0.05Pa, sputtering power 25kW, temperature
The surface deposition thickness of body is the binder course of 100nm, is 316L stainless steel, Cr and tri- kinds of Al in conjunction with layer material；It is in vacuum degree
0.5Pa, sputtering power 30kW, temperature are to continue the inner protective layer that deposition thickness is 8 μm at 50 DEG C, and inner protective layer material is
Tri- kinds of Cu, Zn and Zn-Al；In the case where vacuum degree is 0.2Pa, sputtering power 20kW, temperature are 50 DEG C, continuing deposition thickness is
The transition zone of 300nm, buffer layer material Zn, Zn-Al, ZnO and Al2O3Four kinds；Vacuum degree is 0.6Pa, sputtering power is
32kW, temperature are to continue the external protection that deposition thickness is 3 μm at 40 DEG C, and external protection material is Al2O3, AlN and SiO2Three
Kind.
Embodiment 2
The difference from embodiment 1 is that: the composition of the cleaning solution used when surface preparation are as follows: sodium carbonate 5g/L, it is anhydrous
Calcium oxide 15g/L, sodium hydroxide 10g/L, solvent are water.In addition to cleaning solution composition, other same embodiments of steps and operations condition
1。
Comparative example 1
The difference from embodiment 1 is that: the composition of the cleaning solution used when surface preparation are as follows: sodium carbonate 3g/L, it is anhydrous
Calcium oxide 12g/L, sodium hydroxide 8g/L, solvent are water.In addition to cleaning solution composition, other steps and operations conditions are the same as embodiment 1.
Comparative example 2
The difference from embodiment 1 is that: the composition of the cleaning solution used when surface preparation are as follows: sodium carbonate 12g/L, it is anhydrous
Calcium oxide 24g/L, sodium hydroxide 48g/L, solvent are water.In addition to cleaning solution composition, other same embodiments of steps and operations condition
1。
Salt spray test, Insulation test and magnetic flux test are carried out respectively to the Nd-Fe-B permanent magnet of acquisition, experimental result is such as
Shown in table 1:
The test result that the pairs of Nd-Fe-B permanent magnet performance of 1 cleaning solution group of table influences
As shown in Table 1, when concentration of sodium carbonate is within the scope of 5g/L-10g/L in cleaning solution, dry oxidation calcium concentration is in 15g/
Within the scope of L-20g/L, when naoh concentration is within the scope of 10g/L-40g/L, the Nd-Fe-B permanent magnet of acquisition has preferable
Salt spray resistance.When cleaning solution each component concentration is lower than the lower limit of the range, salt spray resistance is greatly reduced, and illustrates magnet
It is not clean；When cleaning solution each component concentration is higher than the upper limit of the range, salt spray resistance is significantly reduced, explanation
Phenomenon is washed in the presence of crossing, leading to the inside of Nd-Fe-B permanent magnet, there are slight erosions, and then influence its salt spray resistance.
(2) it is cleaned by ultrasonic the influence of time in surface pre-treatment step
Embodiment 3
S1 surface preparation: semi-finished product Nd-Fe-B permanent magnet being placed in cleaning solution and cleans 5min, the composition of cleaning solution are as follows:
Sodium carbonate 10g/L, anhydrous calcium oxide 20g/L, sodium hydroxide 40g/L, solvent are water；It is taken out after cleaning, using 5us/cm
Deionized water rinse 1min；It is taken out after rinsing, is placed in supersonic cleaning machine and is cleaned by ultrasonic 5min, the pH value of ultrasonic water is 6.8；
It is taken out after ultrasonic cleaning, secondary rinsing, rinsing time 1min is carried out using the deionized water of 5 μ s/cm；Taking-up is put into 80 DEG C
5min is dried in drying box.
S2 surface active: the Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, ion activation area
Vacuum degree be 1Pa, use power to be activated for surface of the ion source of 3kW to Nd-Fe-B permanent magnet, activation time
For 3min.
S3 vacuum coating: the Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum degree
It is at 50 DEG C, using the Nd-Fe-B permanent magnetic of vacuum magnetic-control sputtering mode after activation for 0.2Pa, sputtering power 30kW, temperature
The surface deposition thickness of body is the binder course of 500nm, is Ti in conjunction with layer material；Vacuum degree be 1Pa, sputtering power 28kW,
Temperature is to continue the inner protective layer that deposition thickness is 6 μm at 40 DEG C, and inner protective layer material is Sn and Sn-Zn；It is in vacuum degree
1Pa, sputtering power 20kW, temperature are to continue the transition zone that deposition thickness is 1000nm at 40 DEG C, buffer layer material Zn,
Sn-Zn and Al2O3Three kinds；In the case where vacuum degree is 1Pa, sputtering power 30kW, temperature are 40 DEG C, continuing deposition thickness is 6 μm
External protection, external protection material are Cr2O3And CrN.
Embodiment 4
Difference with embodiment 3 is: being cleaned by ultrasonic the time when surface preparation is 0.5min.Except ultrasonic cleaning the time,
Other steps and operations conditions are the same as embodiment 3.
Comparative example 3
Difference with embodiment 3 is: being cleaned by ultrasonic the time when surface preparation is 0.3min.Except ultrasonic cleaning the time,
Other steps and operations conditions are the same as embodiment 3.
Comparative example 4
Difference with embodiment 3 is: being cleaned by ultrasonic the time when surface preparation is 8min.Except ultrasonic cleaning the time,
His steps and operations condition is the same as embodiment 3.
Salt spray test, Insulation test and magnetic flux test are carried out respectively to the Nd-Fe-B permanent magnet of acquisition, experimental result is such as
Shown in table 2:
Table 2 is cleaned by ultrasonic the test result influenced on Nd-Fe-B permanent magnet performance the time
As shown in Table 2, when being cleaned by ultrasonic the time within the scope of 0.5min-5min, the Nd-Fe-B permanent magnet of acquisition has
Preferable salt spray resistance, and salt spray resistance can slightly be improved with the increase of ultrasonic cleaning time.When ultrasonic cleaning
Between be lower than 0.5min when, salt spray resistance is greatly reduced, and illustrates that magnet is not clean；It is higher than when the ultrasonic cleaning time
When 5min, salt spray resistance will not be obviously improved.
(3) in activation step vacuum degree and activation time influence
Embodiment 5
S1 surface preparation: semi-finished product Nd-Fe-B permanent magnet being placed in cleaning solution and cleans 5min, the composition of cleaning solution are as follows:
Sodium carbonate 10g/L, anhydrous calcium oxide 20g/L, sodium hydroxide 40g/L, solvent are water；It is taken out after cleaning, using 7us/cm
Deionized water rinse 1min；It is taken out after rinsing, is placed in supersonic cleaning machine and is cleaned by ultrasonic 5min, the pH value of ultrasonic water is 6.7；
It is taken out after ultrasonic cleaning, secondary rinsing, rinsing time 1min is carried out using the deionized water of 7 μ s/cm；Taking-up is put into 80 DEG C
5min is dried in drying box.
S2 surface active: the Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, ion activation area
Vacuum degree be 0.05Pa, use power to be activated for surface of the ion source of 3kW to Nd-Fe-B permanent magnet, when activation
Between be 3min.
S3 vacuum coating: the Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum degree
It is at 50 DEG C, using the Nd-Fe-B permanent magnet of vacuum magnetic-control sputtering mode after activation for 1Pa, sputtering power 20kW, temperature
Surface deposition thickness be 800nm binder course, in conjunction with layer material be Ti and Al；Vacuum degree is 0.1Pa, sputtering power is
23kW, temperature are to continue the inner protective layer that deposition thickness is 8 μm at 40 DEG C, and inner protective layer material is Al and Si-Al；In vacuum
Degree is 0.5Pa, sputtering power 20kW, temperature are to continue the transition zone that deposition thickness is 1000nm, buffer layer material at 60 DEG C
For SnO2；In the case where vacuum degree is 1Pa, sputtering power 30kW, temperature are 60 DEG C, continue the outer protection that deposition thickness is 0.3 μm
Layer, external protection material are TiO2And TiN.
Embodiment 6
Difference with embodiment 5 is: vacuum degree is 3Pa when surface active.Except the vacuum degree of surface active, other steps
With operating condition with embodiment 5.
Embodiment 7
Difference with embodiment 5 is: activation time is 0.5min when surface active.Except surface active time, other steps
Rapid and operating condition is the same as embodiment 5.
Comparative example 5
Difference with embodiment 5 is: vacuum degree is 0.03Pa when surface active.Except the vacuum degree of surface active, other
Steps and operations condition is the same as embodiment 5.
Comparative example 6
Difference with embodiment 5 is: vacuum degree is 5Pa when surface active.Except the vacuum degree of surface active, other steps
With operating condition with embodiment 5.
Comparative example 7
Difference with embodiment 5 is: activation time is 0.3min when surface active.Except surface active time, other steps
Rapid and operating condition is the same as embodiment 5.
Comparative example 8
Difference with embodiment 5 is: activation time is 5min when surface active.Except surface active time, other steps
With operating condition with embodiment 5.
Salt spray test, Insulation test and magnetic flux test are carried out respectively to the Nd-Fe-B permanent magnet of acquisition, experimental result is such as
Shown in table 3:
The test result that the vacuum degree and activation time of 3 surface active of table influence Nd-Fe-B permanent magnet performance
As shown in Table 3, when the vacuum degree of surface active is within the scope of 0.05Pa-3Pa, activation time is in 0.5min-3min
When in range, the Nd-Fe-B permanent magnet of acquisition has preferable salt spray resistance, and salt spray resistance is with vacuum degree and activation
The increase of time and slightly improve.When vacuum degree is lower than 0.05Pa, salt spray resistance is greatly reduced, this is because ion source
Caused by spread of voltage；When vacuum degree is higher than 3Pa, salt spray resistance is significantly reduced, this is because the electricity of ion source
It flows through caused by big, stability reduction.Further, when activated between be lower than 0.5min when, salt spray resistance is greatly reduced,
Illustrate to activate insufficient；When being higher than 3min between when activated, salt spray resistance is also without being obviously improved.
(4) in vacuum coating step the structure of coating and each thickness degree influence
Embodiment 8
S1 surface preparation and S2 activation step are the same as embodiment 1；
S3 vacuum coating: the Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum degree
It is at 40 DEG C, using the Nd-Fe-B permanent magnetic of vacuum magnetic-control sputtering mode after activation for 0.4Pa, sputtering power 25kW, temperature
The surface deposition thickness of body is the binder course of 1000nm, is 316L stainless steel, tetra- kinds of Cr, Ti and Al in conjunction with layer material；In vacuum
Degree is 0.7Pa, sputtering power 20kW, temperature are to continue the inner protective layer that deposition thickness is 10 μm, inner protective layer material at 40 DEG C
Material is Cu；In the case where vacuum degree is 1Pa, sputtering power 22kW, temperature are 40 DEG C, continue the transition that deposition thickness is 1000nm
Layer, tetra- kinds of buffer layer material Sn, Sn-Zn, Si-Al and Al；Vacuum degree is 1Pa, sputtering power 30kW, temperature are 40 DEG C
Under, continue the external protection that deposition thickness is 6 μm, external protection material is Si3N4。
Embodiment 9
Difference with embodiment 8 is: binder course with a thickness of 10nm.Except joint thickness, other steps and operations items
Part is the same as embodiment 8.
Embodiment 10
Difference with embodiment 8 is: inner protective layer with a thickness of 5 μm.Except inner protective layer thickness, other steps and operations
Condition is the same as embodiment 8.
Embodiment 11
Difference with embodiment 8 is: inner protective layer with a thickness of 1 μm.Except inner protective layer thickness, other steps and operations
Condition is the same as embodiment 8.
Embodiment 12
Difference with embodiment 8 is: transition zone with a thickness of 10nm.Except transition region thickness, other steps and operations items
Part is the same as embodiment 8.
Embodiment 13
Difference with embodiment 8 is: external protection with a thickness of 3 μm.Except protective layer thickness, other steps and operations
Condition is the same as embodiment 8.
Embodiment 14
Difference with embodiment 8 is: external protection with a thickness of 0.3 μm.Except protective layer thickness, other steps and behaviour
Make condition with embodiment 8.
Comparative example 9
Difference with embodiment 8 is: when vacuum coating, not depositing binder course, only Nd-Fe-B permanent magnet after activation
Surface be sequentially depositing inner protective layer, transition zone and external protection.In addition to no binder course, other steps and operations conditions are the same as implementation
Example 8.
Comparative example 10
Difference with embodiment 8 is: when vacuum coating, not depositing transition zone, only Nd-Fe-B permanent magnet after activation
Surface be sequentially depositing binder course, inner protective layer and external protection.In addition to no transition zone, other steps and operations conditions are the same as implementation
Example 8.
Comparative example 11
Difference with embodiment 8 is: when vacuum coating, only the surface of Nd-Fe-B permanent magnet after activation is sequentially depositing
Binder course and external protection.In addition to no inner protective layer and transition zone, other steps and operations conditions are the same as embodiment 8.
Comparative example 12
Difference with embodiment 8 is: when vacuum coating, only the surface deposition of Nd-Fe-B permanent magnet after activation is outer is protected
Sheath.In addition to no binder course, inner protective layer and transition zone, other steps and operations conditions are the same as embodiment 8.
Salt spray test, Insulation test and magnetic flux test are carried out respectively to the Nd-Fe-B permanent magnet of acquisition, experimental result is such as
Shown in table 4:
The test result that the structure of 4 coating of table and each thickness degree influence Nd-Fe-B permanent magnet performance
As shown in Table 4, when the thickness of binder course within the scope of 10nm-1000nm, the thickness of inner protective layer is at 1 μm -10 μm
In range, the thickness of transition zone when the thickness of the inside and outside protective layer of 10nm-1000nm range is in 0.3 μm of -6 μ m, obtain
Nd-Fe-B permanent magnet have preferable salt spray resistance, and salt spray resistance with the increase of binder course and transition region thickness and
It slightly improves, salt spray resistance is significantly improved with the increase of inner protective layer and external protection thickness.
Further, it is also known by table 4, when not depositing binder course, only deposits inner protective layer, transition zone and external protection
When, salt spray resistance is greatly reduced, this is because coating is insecure in conjunction with surface of Nd-Fe-B permanent magnet when lacking binder course
It is caused.When not depositing transition zone, when only depositing binder course, inner protective layer and external protection, due to lacking transition zone, outer protection
Layer is not connected firmly with inner protective layer, and the salt spray resistance of the Nd-Fe-B permanent magnet obtained is also caused to be greatly reduced.When only depositing
When binder course and external protection, salt spray resistance is also undesirable, this is because when only depositing the protective layer of single layer, the protective layer
It should prevent from extraneous salt air corrosion, prevent the corrosion inside magnet again, thus its anti-corrosion capability and pay no attention to
Think.When only depositing external protection, since coating is insecure in conjunction with surface of Nd-Fe-B permanent magnet, the protective layer will be simultaneously in addition
The corrosion inside extraneous and magnet is prevented, salt spray resistance is lower.Therefore, mutually matched binder course, inner protective layer,
Transition zone and external protection structure play a key effect to the salt spray resistance for improving Nd-Fe-B permanent magnet.
(5) in vacuum coating step temperature influence
Embodiment 15
Difference with embodiment 8 is: temperature when vacuum coating is 100 DEG C.In addition to coating temperature, other steps and behaviour
Make condition with embodiment 8.
Comparative example 13
Difference with embodiment 8 is: temperature when vacuum coating is 150 DEG C.In addition to coating temperature, other steps and behaviour
Make condition with embodiment 8.
Comparative example 14
Difference with embodiment 8 is: temperature when vacuum coating is 200 DEG C.In addition to coating temperature, other steps and behaviour
Make condition with embodiment 8.
To embodiment 8, embodiment 15, comparative example 13, comparative example 14, the Nd-Fe-B permanent magnet of acquisition and uncoated
Nd-Fe-B permanent magnet (blank control) is saturated rushes magnetic respectively, magnetic flux is measured after magnetizing, experimental result is as shown in table 5:
The test result that 5 vacuum coating temperature of table influences Nd-Fe-B permanent magnet performance
| Temperature (DEG C) | Saturation rushes magnetic flux (Wb) after magnetic | |
| Embodiment 8 | 40 | 47.64 |
| Embodiment 15 | 100 | 47.61 |
| Comparative example 13 | 150 | 47.27 |
| Comparative example 14 | 200 | 46.92 |
| Blank control | - | 47.62 |
As shown in Table 5, when vacuum coating temperature is higher than 100 DEG C, the Nd-Fe-B permanent magnet of acquisition is after saturation magnetizes
Magnetic flux decreases.When vacuum coating temperature≤100 DEG C, magnetic flux of the Nd-Fe-B permanent magnet of acquisition after saturation magnetizes
It is close with blank control group, it is seen then that the Nd-Fe-B permanent magnetic anti-corrosion insulation plating prepared using preparation method provided by the invention
Layer will not influence the magnetic flux after Nd-Fe-B permanent magnet saturation magnetizes.
(6) with the comparison of existing method
Comparative example 15
Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned using conventional clean liquid, using traditional plating mode, neodymium iron boron forever
Magnet surface nickel plating cupro-nickel.
Comparative example 16
Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned using conventional clean liquid, using traditional plating mode, neodymium iron boron forever
Magnet surface nickel plating cupro-nickel, and further composite electrophoresis epoxy coating.
Comparative example 17
Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned using conventional clean liquid, at 200 DEG C, using vacuum magnetic-control sputtering side
Formula is aluminized in surface of Nd-Fe-B permanent magnet.
Comparative example 18
Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned using conventional clean liquid, at 200 DEG C, using vacuum magnetic-control sputtering side
Formula is aluminized in surface of Nd-Fe-B permanent magnet, and further composite electrophoresis epoxy coating.
To embodiment 1, embodiment 3, embodiment 5, embodiment 8, comparative example 15, comparative example 16, comparative example 17 and comparative example
It is as shown in table 6 that 18 Nd-Fe-B permanent magnets obtained carry out salt spray test, Insulation test and magnetic flux test, comparison result respectively:
The comparison of table 6 preparation method provided by the invention and existing method
As shown in Table 6, it using preparation method provided by the invention, is obtained using different coating materials and plating conditions preparation
The Nd-Fe-B permanent magnet obtained, all has stronger salt spray resistance, and the super 1200h of salt-fog resistant time is existing much higher than other
There is preparation method.Moreover, the Nd-Fe-B permanent magnet prepared using preparation method provided by the invention, coating are inherently had
There is preferable insulation performance, be not necessarily to composite electrophoresis epoxy coating, preparation process is simpler, cost is lower and more environmentally friendly.
Claims (5)
1. a kind of preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating, which comprises the steps of:
Surface preparation: cleaning semi-finished product surface of Nd-Fe-B permanent magnet is dried after removing pollutant；
Surface active: the Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, using ion source to described
The surface of Nd-Fe-B permanent magnet is activated；
Vacuum coating: the vacuum coating area that the Nd-Fe-B permanent magnet after activation moves to vacuum coating equipment is adopted at≤100 DEG C
Binder course, inner protective layer, transition zone are sequentially depositing with the surface of the Nd-Fe-B permanent magnet of vacuum magnetic-control sputtering mode after activation
And external protection；The binder course with a thickness of 10nm-1000nm, the inner protective layer with a thickness of 1 μm -10 μm, the mistake
Cross layer with a thickness of 10nm-1000nm, the external protection with a thickness of 0.3 μm -6 μm；The material of the binder course be selected from Al,
One of Cr, Ti or stainless steel or a variety of；The material of the inner protective layer be selected from Sn, Zn, Cu, Al, Si-Al, Zn-Al or
One of Sn-Zn or a variety of；The material of the transition zone is selected from Sn, Zn, Al, Si-Al, Zn-Al, Sn-Zn, SnO2, ZnO or
Al2O3One of or it is a variety of；The material of the external protection is selected from Al2O3、AlN、Cr2O3、TiO2、SiO2、Si3N4, TiN or
One of CrN or a variety of.
2. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1, which is characterized in that in the table
In the pre-treatment step of face, the specific steps of cleaning semi-finished product surface of Nd-Fe-B permanent magnet include: by semi-finished product Nd-Fe-B permanent magnet
It is placed in cleaning solution and cleans；It takes out after cleaning, is rinsed using deionized water；It takes out, is placed in supersonic cleaning machine after rinsing
Ultrasonic cleaning；It is taken out after ultrasonic cleaning, secondary rinsing is carried out using deionized water.
3. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 2, which is characterized in that the cleaning
The composition of liquid are as follows: sodium carbonate 5g/L-10g/L, anhydrous calcium oxide 15g/L-20g/L, sodium hydroxide 10g/L-40g/L, solvent are
Water；The ultrasonic cleaning time is 0.5min-5min.
4. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1, it is characterised in that: in the table
In the activation step of face, the vacuum degree in the ion activation area is 0.05Pa-3Pa, and the power of the ion source is 3kW-7kW, living
The change time is 0.5min-3min.
5. the Nd-Fe-B permanent magnet that a kind of surface has anti-corrosion insulation coating, it is characterised in that: the anti-corrosion insulation coating uses
Preparation method according to any one of claims 1-4 prepares.
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| CN107675134A (en) * | 2017-09-26 | 2018-02-09 | 湖北汽车工业学院 | A kind of sintered Nd-Fe-B permanent magnet surface nitride composite deposite and preparation method |
| CN109554677A (en) * | 2018-12-26 | 2019-04-02 | 湖北永磁磁材科技有限公司 | A kind of sintered Nd-Fe-B permanent magnet surface Zinc-tin alloy coating and preparation method thereof |
| CN110129733B (en) * | 2019-06-19 | 2020-11-10 | 东北大学 | Sintered neodymium-iron-boron magnet with composite film layer and preparation method thereof |
| CN114928187A (en) * | 2019-12-24 | 2022-08-19 | 深之蓝海洋科技股份有限公司 | Permanent magnet rotor structure of underwater motor, underwater motor and underwater equipment |
| CN116497325A (en) * | 2023-03-29 | 2023-07-28 | 广东省科学院资源利用与稀土开发研究所 | Surface protection modification method for neodymium-iron-boron magnet for magnetic squeezing |
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