CN107419231A - The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating and the Nd-Fe-B permanent magnet with the coating - Google Patents
The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating and the Nd-Fe-B permanent magnet with the coating Download PDFInfo
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- CN107419231A CN107419231A CN201710616213.0A CN201710616213A CN107419231A CN 107419231 A CN107419231 A CN 107419231A CN 201710616213 A CN201710616213 A CN 201710616213A CN 107419231 A CN107419231 A CN 107419231A
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 170
- 239000011248 coating agent Substances 0.000 title claims abstract description 75
- 238000000576 coating method Methods 0.000 title claims abstract description 75
- 238000005260 corrosion Methods 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 238000009413 insulation Methods 0.000 title claims abstract description 42
- 238000001994 activation Methods 0.000 claims abstract description 61
- 239000011241 protective layer Substances 0.000 claims abstract description 55
- 230000004913 activation Effects 0.000 claims abstract description 50
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 50
- 239000011230 binding agent Substances 0.000 claims abstract description 36
- 238000004544 sputter deposition Methods 0.000 claims abstract description 34
- 230000007704 transition Effects 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000011265 semifinished product Substances 0.000 claims abstract description 23
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 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 60
- 238000004140 cleaning Methods 0.000 claims description 53
- 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
- 239000012530 fluid Substances 0.000 claims description 28
- 239000010410 layer Substances 0.000 claims description 28
- 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
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052718 tin Inorganic materials 0.000 claims description 12
- 238000004506 ultrasonic cleaning Methods 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
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 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
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910017083 AlN Inorganic materials 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 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
- 239000010935 stainless steel Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 230000004907 flux Effects 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 14
- 150000003839 salts Chemical class 0.000 description 33
- 239000007921 spray Substances 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 27
- 238000012360 testing method Methods 0.000 description 24
- 238000000034 method Methods 0.000 description 18
- 230000007797 corrosion Effects 0.000 description 15
- 238000007747 plating Methods 0.000 description 12
- 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
- 238000005516 engineering process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000002421 anti-septic effect Effects 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 230000008021 deposition Effects 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
- 230000009467 reduction Effects 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
- 230000007423 decrease Effects 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
- 239000000047 product 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
- 230000000903 blocking effect 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
- 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
- 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
- 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
- 238000010998 test method Methods 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
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 on the premise of Nd-Fe-B permanent magnet magnetic flux is not influenceed.The preparation method comprises the following steps：Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned, is dried after removing pollutant；The Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, activation process is carried out to the surface of the Nd-Fe-B permanent magnet using ion gun；Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, at≤100 DEG C, binder course, inner protective layer, transition zone and external protection are sequentially depositing using the surface of the Nd-Fe-B permanent magnet of vacuum magnetic-control sputtering mode after activation.
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-corrosion
The preparation method of insulating blanket and the Nd-Fe-B permanent magnet with the coating.
Background technology
Nd-Fe-B permanent magnet material (chemical name NdFeB) belongs to third generation rare earth permanent magnet, because with high remanent magnetism, high-coercive force and
The characteristics such as high energy product, it is widely used in New-energy electric vehicle, magneto used for wind power generation, magnetic suspension, unmanned plane etc.
Numerous Chaoyang industries.Although Nd-Fe-B permanent magnet material has excellent magnetic property, but its corrosion resistance is poor, thus, existing
Have in technology, generally plate overcoat in neodymium-iron-boron permanent magnetic material surface, to avoid causing the reduction of its magnetic property because magnet corrodes,
Extend its service life.
At present, the anti-corrosion method of Nd-Fe-B permanent magnet material has a variety of, and traditional method is wet using plating or chemical plating etc.
Method technique surface of Nd-Fe-B permanent magnet plated with nickel, zinc or nickel-copper-nickel composite bed, but use this wet processing, once plating
Liquid is penetrated into the internal void of Nd-Fe-B permanent magnet, can cause the accelerated corrosion of permanent magnet on the contrary.With surface coating technology
Development, the method that overcoat has been plated in neodymium-iron-boron permanent magnetic material surface using dry process such as Vacuum Depositions 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, it 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,
This method still suffers from some shortcomings：(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 through high-temperature process can exist Nd-Fe-B permanent magnet magnetic flux reduction potential risk；(2) existing method is led to
Individual layer aluminium film only often is plated on the surface of Nd-Fe-B permanent magnet, is directly in conjunction with pinning effect between coating and Nd-Fe-B permanent magnet
On the weak side, the fastness and anticorrosion effect of coating can decrease.
Therefore, how on the premise of Nd-Fe-B permanent magnet magnetic flux is not influenceed, fastness and anticorrosion effect are prepared more
Good Nd-Fe-B permanent magnetic anti-corrosion insulation coating, it is a current technical problem for being badly in need of solving.
The content of the invention
The present invention is directed to above-mentioned technical problem, proposes a kind of preparation method and tool 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 on the premise of Nd-Fe-B permanent magnet magnetic flux is not influenceed
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 is：
The present invention proposes a kind of preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating, comprises the following steps：
Surface preparation：Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned, 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 gun pair
The surface of the Nd-Fe-B permanent magnet carries out activation process；
Vacuum coating：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 thickness of the binder course is 10nm-1000nm, the thickness of the inner protective layer is 1 μm -10 μm,
The thickness of the transition zone is 10nm-1000nm, and the thickness of the external protection is 0.3 μm -6 μm.
Preferably, one or more of the material of the binder course in Al, Cr, Ti or stainless steel.
Preferably, the one kind of the material of the inner protective layer in Sn, Zn, Cu, Al, Si-Al, Zn-Al or Sn-Zn
It is or 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
Al2O3In one or more.
Preferably, the material of the external protection is selected from Al2O3、AlN、Cr2O3、TiO2、SiO2、Si3N4, TiN or CrN
In one or more.
Preferably, in the surface pre-treatment step, the specific steps of semi-finished product surface of Nd-Fe-B permanent magnet are cleaned
Including：Semi-finished product Nd-Fe-B permanent magnet is placed in cleaning fluid and cleaned；Take out after cleaning, rinsed using deionized water；Drift
Taken out after washing, be placed in supersonic cleaning machine and be cleaned by ultrasonic；Taken out after ultrasonic cleaning, secondary rinsing is carried out using deionized water.
Preferably, the composition of the cleaning fluid is：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, in the activation step, the vacuum in the ion activation area is 0.05Pa-3Pa, described
The power of ion gun is 3kW-7kW, soak time 0.5min-3min.
Present invention also offers the Nd-Fe-B permanent magnet that a kind of surface has anti-corrosion insulation coating, the anti-corrosion insulation coating
Prepared using the preparation method described in any one technical scheme as described above.
Compared with prior art, the advantages and positive effects of the present invention are：
1st, the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention, it utilizes vacuum at≤100 DEG C
The coating of surface of Nd-Fe-B permanent magnet deposition sandwich construction of the magnetron sputtering mode after ion gun activation, the coating of acquisition have
Good Corrosion Protection；
2nd, 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 influenceed, while also there is insulation characterisitic, disclosure satisfy that
Multiple functions requirement of the various magneto fields to Nd-Fe-B permanent magnet coating, the scope of application are more extensive.
Brief description of the drawings
The surface that Fig. 1 is provided by the embodiment of the present invention has the structural representation of the Nd-Fe-B permanent magnet of anti-corrosion insulation coating
Figure；
In figure, 1, external protection；2nd, transition zone；3rd, inner protective layer；4th, binder course；5th, semi-finished product Nd-Fe-B permanent magnet.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
The embodiments of the invention provide a kind of preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating, comprise the following steps：
S1 surface preparations：Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned, is dried after removing pollutant.
In this step, the pollutant of surface of Nd-Fe-B permanent magnet, especially grease etc. are removed by cleaning, after being advantageous to
It is continuous to carry out plated film.It should be noted that during cleaning, it is totally standard that surface contaminant, which is removed,.
Further, this step is dried after cleaning, can be removed the moisture inside Nd-Fe-B permanent magnet, be avoided shadow
Ring antiseptic effect.It should be noted that in drying, drying temperature is selected to be advisable for 50 DEG C -120 DEG C, 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 due to：Drying temperature is less than 50 DEG C, its
Drying effect is poor, has moisture and penetrates into inside Nd-Fe-B permanent magnet, influences antiseptic effect；And drying temperature is higher than 120 DEG C, deposit
Influenceing the potential risk of 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., you can ensure that Nd-Fe-B permanent magnet is fully dried, can avoid drying again
Overlong time causes to waste.It is understood that those skilled in the art can be according to the moistening of Nd-Fe-B permanent magnet after cleaning
Situation, drying condition is specifically adjusted, for example, when the drying temperature of selection is slightly higher, drying time can suitably shorten；The drying of selection
When temperature is slightly lower, drying time can proper extension.
In addition it is also necessary to explanation, the 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 actives：The Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, using ion gun
Activation process is carried out to the surface of the Nd-Fe-B permanent magnet.
In this step, activation process is carried out to the surface of Nd-Fe-B permanent magnet using ion gun, neodymium iron boron can be made forever
The arrow of magnet surface can improve 1 magnitude, reduce subsequent plating layer and required energy barrier is combined with surface of Nd-Fe-B permanent magnet, favorably
In the combination of subsequent plating layer, the fastness of coating is improved.
S3 vacuum coatings：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.
It is normal compared to vacuum magnetic-control sputtering in this step, it is necessary to which explanation, carries out vacuum coating at≤100 DEG C
More than 200 DEG C of the high-temperature process used, can avoid 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 passes through activation process, and plates binder course during plated film first to strengthen coating and neodymium iron
The combination of boron permanent magnet surfaces, thus, vacuum coating is carried out at≤100 DEG C, remains able to ensure the jail that coating combines
Solidity.It is understood that those skilled in the art can be specifically chosen suitable according to the specific material and thickness requirement of coating
Temperature, such as：Temperature during 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,
It should also be noted that, sputter temperature during vacuum coating can be regulated and controled by the way of water cooling.
Further, the coating in this step includes binder course, inner protective layer, transition zone and external protection, wherein, with reference to
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 a part of blocking Nd-Fe-B permanent magnet internal flaw；Transition zone master
Play a part 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 sandwich construction used in rapid is more firm, and employs inner protective layer
It is more preferable with two layers of overcoat of external protection, anticorrosion effect.
In addition it is also necessary to explanation, apart from the temperature, the other conditions that vacuum magnetic-control sputtering uses and existing vacuum magnetic control
Sputtering condition is similar, such as：The vacuum in vacuum coating area is 0.05Pa-1Pa, sputtering power 15kW-40kW, it is possible to understand that
, those skilled in the art specifically chosen suitable vacuum and can be splashed according to the specific material and thickness requirement of coating
Power is penetrated, such as：Vacuum 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..During vacuum coating, because 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 zones can use different splash
Penetrate temperature, vacuum and sputtering power.
The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention, it utilizes Vacuum Magnetic at≤100 DEG C
The coating of surface of Nd-Fe-B permanent magnet deposition sandwich construction of the sputtering mode after ion gun activation is controlled, the coating of acquisition has good
Good Corrosion Protection.Moreover, prepared using the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating provided by the invention
Coating, while with good Corrosion Protection, do not influence Nd-Fe-B permanent magnet magnetic flux, while also have insulation special
Property, it disclosure satisfy that various magneto fields are required the multiple functions of Nd-Fe-B permanent magnet coating, the scope of application is more extensive.
In a preferred embodiment, the thickness of the binder course is 10nm-1000nm, and the thickness of the inner protective layer is 1 μ
M-10 μm, the thickness of the transition zone is 10nm-1000nm, and the thickness of the external protection is 0.3 μm -6 μm.It is preferred real at this
Apply in example, further define the thickness of binder course, inner protective layer, transition zone and external protection, the thickness range is optimal model
Enclose, 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 of coating is influenceed, only when the thickness of binder course, inner protective layer, transition zone and external protection is mutually matched,
Can obtain not only had had good corrosion resistance but also the coating being firmly combined with.It is understood that those skilled in the art can basis
The thickness of the specifically chosen each layer of requirement for anticorrosion of coating, such as：The thickness of binder course can be 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 10nm, 50nm, 100nm, 300nm, 500nm, 700nm, 1000nm etc., and the thickness of external protection can be with
For 0.3 μm, 0.5 μm, 1 μm, 2 μm, 4 μm, 6 μm etc..
In a preferred embodiment, one or more of the material of the binder course in Al, Cr, Ti or stainless steel.
In the preferred embodiment, the material of binder course is further defined, these materials have stronger parent with Nd-Fe-B permanent magnet
And property, be advantageous to improve coating fastness.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
In one or more.In the preferred embodiment, the material of inner protective layer is further defined, these materials have stronger
The performance of decay resistance and closure magnet surface hole, be advantageous to improve the corrosion resistance of 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 Al2O3In one or more.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 advantageous 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 or more in TiN or CrN.In the preferred embodiment, the material of external protection is further defined, these materials tool
There are stronger decay resistance and insulating properties, be advantageous to improve the corrosion resistance and insulating properties of coating.It is understood that this
Art personnel 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：Semi-finished product Nd-Fe-B permanent magnet is placed in cleaning fluid and cleaned；Taken out after cleaning, using deionized water
Rinsing；Taken out after rinsing, be placed in supersonic cleaning machine and be cleaned by ultrasonic；Take out, 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, it is cleaned by ultrasonic and rinses twice, can ensures the pollutant removal of surface of Nd-Fe-B permanent magnet is clean.
In further preferred embodiments, the composition of the cleaning fluid is：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
Select in embodiment, further define the composition of cleaning fluid and the time of ultrasonic cleaning, the composition of the cleaning fluid and ultrasonic cleaning
Time is optimized scope, can cause necessarily to adversely affect when beyond this scope.Such as：Formed for cleaning fluid, when each
When the concentration of component is less 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, surface of Nd-Fe-B permanent magnet is caused
Slight erosion, influence coating antiseptic effect.It is understood that those skilled in the art can be according to surface of Nd-Fe-B permanent magnet
Pollution level, specifically chosen suitable cleaning fluid 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 being cleaned by ultrasonic the time, when being cleaned by ultrasonic the time less than 0.5 minute, its cleaning performance may not
Substantially, when being cleaned by ultrasonic the time higher than 5 minutes, its cleaning quality will not also obtain higher lifting, can cause the energy on the contrary
Waste.It is understood that those skilled in the art can be according to the pollution level of surface of Nd-Fe-B permanent magnet, specifically chosen conjunction
The suitable ultrasonic cleaning time, such as：0.5min, 1min, 3min, 5min etc..Furthermore, it is necessary to explanation, except cleaning fluid forms
Be cleaned by ultrasonic outside the time, in cleaning process, the time cleaned using cleaning fluid is advisable in 1min-5min, is adopted during rinsing
It is advisable with 1 μ s/cm-10 μ s/cm deionized water, 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, is washed with cleaning up, occurring without
Phenomenon and the saving energy are standard.
In a preferred embodiment, in the activation step, the vacuum in the ion activation area is 0.05Pa-
3Pa, the power of the ion gun is 3kW-7kW, soak time 0.5min-3min.In the preferred embodiment, further limit
Determine surface active condition, the surface active condition is optimal conditions, can cause necessarily to adversely affect when beyond this scope,
Only when activating vacuum, ion source power and soak time mutual cooperation, best surface-activation effect could be obtained.Example
Such as：For vacuum, when vacuum is less than 0.05Pa, ion source voltage potentially unstable, surface-activation effect is influenceed；Surely
When reciprocal of duty cycle is higher than 3Pa, the electric current of ion gun is excessive, and stability may also reduce.For soak time, upon activation between be less than
During 0.5min, it is understood that there may be activate insufficient phenomenon；And activating 3min can ensure that activation is abundant, when continuing to extend activation
Between, activation effect will not be also improved, causes the waste of the energy afterwards on the contrary.It is understood that those skilled in the art can root
According to coating material and requirement for anticorrosion, specifically chosen suitable activation condition, such as：Vacuum can be 0.05Pa, 0.1Pa,
0.5Pa, 1Pa, 2Pa, 3Pa etc., ion source power can be 3kW, 5kW, 7kW etc., soak time can be 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 the preparation method described in any of the above-described embodiment.The Nd-Fe-B permanent magnetic
Body, there is good Corrosion Protection and insulating properties, its remanent magnetism amount after magnetizing is higher, applied widely.
In order to become apparent from introducing the preparation for the Nd-Fe-B permanent magnetic anti-corrosion insulation coating that the embodiment of the present invention is provided in detail
Method and the 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 through chamfer polishing after machining finishes
The semi-finished product Nd-Fe-B permanent magnet that the trade mark is 45H, specification is 50mm × 23mm × 2.8mm.In addition, the Nd-Fe-B permanent magnetic to 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 standards；Insulating properties method of testing is：
In copper electrodes of the upper and lower surface covering with wire of permanent magnet, two wires, general-purpose are contacted simultaneously with two indicators of universal meter
The resistance value of table is the insulation numerical value of permanent magnet, and insulation number range is from infinity to zero；Magnetic flux uses Chinese metering section
Graduate HT707 intelligence fluxmeter is learned to be detected.
Investigate, and illustrate respectively below for the major parameter and operating condition being related in each step：
(1) influence that cleaning fluid forms in surface pre-treatment step
Embodiment 1
S1 surface preparations：Semi-finished product Nd-Fe-B permanent magnet is placed in cleaning fluid and cleans 5min, the composition of cleaning fluid is：
Sodium carbonate 10g/L, anhydrous calcium oxide 20g/L, sodium hydroxide 40g/L, solvent are water；Taken out after cleaning, using 10us/cm
Deionized water rinsing 1min；Taken out after rinsing, be placed in supersonic cleaning machine and be cleaned by ultrasonic 5min, the pH value of ultrasonic water is 6.5；
Taken out after ultrasonic cleaning, secondary rinsing, rinsing time 1min are carried out using 10 μ s/cm deionized water；Taking-up is put into 80 DEG C
Drying baker in drying 5min.
S2 surface actives：The Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, ion activation area
Vacuum be 1Pa, use power to carry out activation process, soak time to the surface of Nd-Fe-B permanent magnet for 3kW ion gun
For 3min.
S3 vacuum coatings：Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum
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 deposit thickness of body is 100nm binder course, is tri- kinds of 316L stainless steels, Cr and Al with reference to layer material；It is in vacuum
0.5Pa, sputtering power 30kW, temperature are at 50 DEG C, continue the inner protective layer that deposit thickness is 8 μm, and inner protective layer material is
Tri- kinds of Cu, Zn and Zn-Al；In the case where vacuum is 0.2Pa, sputtering power 20kW, temperature are 50 DEG C, continuing deposit thickness is
300nm transition zone, buffer layer material Zn, Zn-Al, ZnO and Al2O3Four kinds；Vacuum be 0.6Pa, sputtering power be
32kW, temperature are at 40 DEG C, continue the external protection that deposit thickness is 3 μm, external protection material is Al2O3, AlN and SiO2Three
Kind.
Embodiment 2
Difference with embodiment 1 is：The composition of the cleaning fluid used during surface preparation for：Sodium carbonate 5g/L, it is anhydrous
Calcium oxide 15g/L, sodium hydroxide 10g/L, solvent are water.In addition to cleaning fluid forms, other same embodiments of steps and operations condition
1。
Comparative example 1
Difference with embodiment 1 is：The composition of the cleaning fluid used during surface preparation for：Sodium carbonate 3g/L, it is anhydrous
Calcium oxide 12g/L, sodium hydroxide 8g/L, solvent are water.In addition to cleaning fluid forms, other steps and operations conditions are the same as embodiment 1.
Comparative example 2
Difference with embodiment 1 is：The composition of the cleaning fluid used during surface preparation for：Sodium carbonate 12g/L, it is anhydrous
Calcium oxide 24g/L, sodium hydroxide 48g/L, solvent are water.In addition to cleaning fluid forms, 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 cleaning fluid of table 1 forms the test result to Nd-Fe-B permanent magnet performance impact
As shown in Table 1, when concentration of sodium carbonate is in the range of 5g/L-10g/L in cleaning fluid, dry oxidation calcium concentration is in 15g/
In the range of L-20g/L, when naoh concentration is in the range of 10g/L-40g/L, the Nd-Fe-B permanent magnet of acquisition has preferably
Salt spray resistance.When cleaning fluid each component concentration is less than the lower limit of the scope, its salt spray resistance is greatly reduced, and illustrates magnet
Do not clean clean；When cleaning fluid each component concentration is higher than the upper limit of the scope, its salt spray resistance is significantly reduced, explanation
Phenomenon is washed in the presence of crossing, causes the inside of Nd-Fe-B permanent magnet slight erosion to be present, 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 preparations：Semi-finished product Nd-Fe-B permanent magnet is placed in cleaning fluid and cleans 5min, the composition of cleaning fluid is：
Sodium carbonate 10g/L, anhydrous calcium oxide 20g/L, sodium hydroxide 40g/L, solvent are water；Taken out after cleaning, using 5us/cm
Deionized water rinsing 1min；Taken out after rinsing, be placed in supersonic cleaning machine and be cleaned by ultrasonic 5min, the pH value of ultrasonic water is 6.8；
Taken out after ultrasonic cleaning, secondary rinsing, rinsing time 1min are carried out using 5 μ s/cm deionized water；Taking-up is put into 80 DEG C
Drying 5min in drying baker.
S2 surface actives：The Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, ion activation area
Vacuum be 1Pa, use power to carry out activation process, soak time to the surface of Nd-Fe-B permanent magnet for 3kW ion gun
For 3min.
S3 vacuum coatings：Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum
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 deposit thickness of body is 500nm binder course, is Ti with reference to layer material；Vacuum be 1Pa, sputtering power 28kW,
Temperature is at 40 DEG C, continues the inner protective layer that deposit thickness is 6 μm, inner protective layer material is Sn and Sn-Zn；It is in vacuum
1Pa, sputtering power 20kW, temperature are the transition zone that continuation deposit thickness is 1000nm at 40 DEG C, buffer layer material Zn,
Sn-Zn and Al2O3Three kinds；In the case where vacuum is 1Pa, sputtering power 30kW, temperature are 40 DEG C, it is 6 μm to continue deposit thickness
External protection, external protection material are Cr2O3And CrN.
Embodiment 4
Difference with embodiment 3 is：It is 0.5min to be cleaned by ultrasonic the time during surface preparation.Except be cleaned by ultrasonic the time,
Other steps and operations conditions are the same as embodiment 3.
Comparative example 3
Difference with embodiment 3 is：It is 0.3min to be cleaned by ultrasonic the time during surface preparation.Except be cleaned by ultrasonic the time,
Other steps and operations conditions are the same as embodiment 3.
Comparative example 4
Difference with embodiment 3 is：It is 8min to be cleaned by ultrasonic the time during surface preparation.Except be cleaned by ultrasonic the time, its
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 test result of the time to Nd-Fe-B permanent magnet performance impact
As shown in Table 2, when being cleaned by ultrasonic the time in the range of 0.5min-5min, the Nd-Fe-B permanent magnet of acquisition has
Preferable salt spray resistance, and salt spray resistance can slightly improve with the increase for being cleaned by ultrasonic the time.When being cleaned by ultrasonic
Between when being less than 0.5min, its salt spray resistance is greatly reduced, and it is clean to illustrate that magnet does not clean；It is higher than when being cleaned by ultrasonic the time
During 5min, its salt spray resistance will not be also obviously improved.
(3) in activation step vacuum and soak time influence
Embodiment 5
S1 surface preparations：Semi-finished product Nd-Fe-B permanent magnet is placed in cleaning fluid and cleans 5min, the composition of cleaning fluid is：
Sodium carbonate 10g/L, anhydrous calcium oxide 20g/L, sodium hydroxide 40g/L, solvent are water；Taken out after cleaning, using 7us/cm
Deionized water rinsing 1min；Taken out after rinsing, be placed in supersonic cleaning machine and be cleaned by ultrasonic 5min, the pH value of ultrasonic water is 6.7；
Taken out after ultrasonic cleaning, secondary rinsing, rinsing time 1min are carried out using 7 μ s/cm deionized water；Taking-up is put into 80 DEG C
Drying 5min in drying baker.
S2 surface actives：The Nd-Fe-B permanent magnet of drying is placed in the ion activation area of vacuum coating equipment, ion activation area
Vacuum be 0.05Pa, use power to carry out activation process to the surface of Nd-Fe-B permanent magnet for 3kW ion gun, during activation
Between be 3min.
S3 vacuum coatings：Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum
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 deposit thickness be 800nm binder course, be Ti and Al with reference to layer material；Vacuum be 0.1Pa, sputtering power be
23kW, temperature are at 40 DEG C, continue the inner protective layer that deposit thickness is 8 μm, inner protective layer material is Al and Si-Al；In vacuum
It is at 60 DEG C to spend for 0.5Pa, sputtering power 20kW, temperature, continues the transition zone that deposit thickness is 1000nm, buffer layer material
For SnO2；In the case where vacuum is 1Pa, sputtering power 30kW, temperature are 60 DEG C, continue the outer protection that deposit thickness is 0.3 μm
Layer, external protection material is TiO2And TiN.
Embodiment 6
Difference with embodiment 5 is：Vacuum is 3Pa during surface active.Except the vacuum of surface active, other steps
With operating condition with embodiment 5.
Embodiment 7
Difference with embodiment 5 is：Soak time is 0.5min during 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 is 0.03Pa during surface active.Except the vacuum of surface active, other
Steps and operations condition is the same as embodiment 5.
Comparative example 6
Difference with embodiment 5 is：Vacuum is 5Pa during surface active.Except the vacuum of surface active, other steps
With operating condition with embodiment 5.
Comparative example 7
Difference with embodiment 5 is：Soak time is 0.3min during 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：Soak time is 5min during 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 of the vacuum of the surface active of table 3 and soak time to Nd-Fe-B permanent magnet performance impact
As shown in Table 3, when the vacuum of surface active is in the range of 0.05Pa-3Pa, soak time is in 0.5min-3min
In the range of when, the Nd-Fe-B permanent magnet of acquisition has preferable salt spray resistance, and salt spray resistance is with vacuum and activation
The increase of time and slightly improve.When vacuum is less than 0.05Pa, its salt spray resistance is greatly reduced, and this is due to ion gun
Caused by spread of voltage；When vacuum is higher than 3Pa, its salt spray resistance is significantly reduced, and this is due to the electricity of ion gun
Flow through greatly, caused by stability reduction.Further, upon activation between when being less than 0.5min, its salt spray resistance is greatly reduced,
Illustrate that activation is insufficient；When being higher than 3min between upon activation, its 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 preparations and S2 activation steps are the same as embodiment 1；
S3 vacuum coatings：Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, in vacuum
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 deposit thickness of body is 1000nm binder course, is 316L stainless steels, tetra- kinds of Cr, Ti and Al with reference to layer material；In vacuum
It is at 40 DEG C to spend for 0.7Pa, sputtering power 20kW, temperature, continues the inner protective layer that deposit thickness is 10 μm, inner protective layer material
Expect for Cu；In the case where vacuum is 1Pa, sputtering power 22kW, temperature are 40 DEG C, continue the transition that deposit thickness is 1000nm
Layer, tetra- kinds of buffer layer material Sn, Sn-Zn, Si-Al and Al；Vacuum be 1Pa, sputtering power 30kW, temperature be 40 DEG C
Under, continue the external protection that deposit thickness is 6 μm, external protection material is Si3N4。
Embodiment 9
Difference with embodiment 8 is：The thickness of binder course is 10nm.Except joint thickness, other steps and operations bars
Part is the same as embodiment 8.
Embodiment 10
Difference with embodiment 8 is：The thickness of inner protective layer is 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：The thickness of inner protective layer is 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：The thickness of transition zone is 10nm.Except transition region thickness, other steps and operations bars
Part is the same as embodiment 8.
Embodiment 13
Difference with embodiment 8 is：The thickness of external protection is 3 μm.Except protective layer thickness, other steps and operations
Condition is the same as embodiment 8.
Embodiment 14
Difference with embodiment 8 is：The thickness of external protection is 0.3 μm.Except protective layer thickness, other steps and behaviour
Make condition with embodiment 8.
Comparative example 9
Difference with embodiment 8 is：During vacuum coating, binder course, Nd-Fe-B permanent magnet only after activation are not deposited
Surface be sequentially depositing inner protective layer, transition zone and external protection.In addition to without binder course, other steps and operations conditions are the same as implementation
Example 8.
Comparative example 10
Difference with embodiment 8 is：During vacuum coating, transition zone, Nd-Fe-B permanent magnet only after activation are not deposited
Surface be sequentially depositing binder course, inner protective layer and external protection.In addition to without transition zone, other steps and operations conditions are the same as implementation
Example 8.
Comparative example 11
Difference with embodiment 8 is：During vacuum coating, the surface of Nd-Fe-B permanent magnet only after activation is sequentially depositing
Binder course and external protection.In addition to without 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：During vacuum coating, the surface deposition of Nd-Fe-B permanent magnet only after activation is outer to protect
Sheath.In addition to without 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 of the structure of the coating of table 4 and each thickness degree to Nd-Fe-B permanent magnet performance impact
As shown in Table 4, when binder course thickness in the range of 10nm-1000nm, the thickness of inner protective layer is at 1 μm -10 μm
In the range of, the thickness of transition zone in the range of 10nm-1000nm, the thickness of external protection in 0.3 μm of -6 μ m when, obtain
Nd-Fe-B permanent magnet there is preferable salt spray resistance, and salt spray resistance with the increase of binder course and transition region thickness and
Slightly improve, salt spray resistance significantly improves with the increase of inner protective layer and external protection thickness.
Further, also known by table 4, when not depositing binder course, only deposit inner protective layer, transition zone and external protection
When, its salt spray resistance is greatly reduced, and this is due to when lacking binder course, and coating is combined insecure with surface of Nd-Fe-B permanent magnet
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
The salt spray resistance that layer is connected insecure, also to cause to obtain Nd-Fe-B permanent magnet with inner protective layer is greatly reduced.When only depositing
When binder course and external protection, its salt spray resistance is also undesirable, and this is due to protective layer when only depositing the protective layer of individual layer
The salt air corrosion from the external world should be prevented, prevents the corrosion inside magnet again, thus its anti-corrosion capability and is paid no attention to
Think.When only depositing external protection, because coating is combined with surface of Nd-Fe-B permanent magnet insecure, the protective layer will be simultaneously in addition
Prevent lower from the extraneous corrosion with inside magnet, its salt spray resistance.Therefore, the binder course of mutual cooperation, inner protective layer,
Transition zone and external protection structure, the salt spray resistance for improving Nd-Fe-B permanent magnet is played a key effect.
(5) in vacuum coating step temperature influence
Embodiment 15
Difference with embodiment 8 is：Temperature during 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 during 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 during 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 it is uncoated
Saturation rushes magnetic to Nd-Fe-B permanent magnet (blank control) respectively, magnetic flux is measured after magnetizing, experimental result is as shown in table 5：
Test result of the vacuum coating temperature of table 5 to Nd-Fe-B permanent magnet performance impact
| 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, the magnetic flux of the Nd-Fe-B permanent magnet of acquisition after saturation magnetizes
Approached 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 does not interfere with the magnetic flux after Nd-Fe-B permanent magnet saturation magnetizes.
(6) with the contrast 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, in 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, in 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, 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, 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, comparative result respectively：
The contrast of 6 preparation method provided by the invention of table and existing method
As shown in Table 6, using preparation method provided by the invention, prepared and obtained using different coating materials and plating conditions
The Nd-Fe-B permanent magnet obtained, it is respectively provided with stronger salt spray resistance, and the super 1200h of salt-fog resistant time is existing far above others
There is preparation method.Moreover, the Nd-Fe-B permanent magnet prepared using preparation method provided by the invention, its coating inherently has
There are preferable insulating properties, without composite electrophoresis epoxy coating, preparation technology is simpler, cost is lower and more environmentally friendly.
Claims (10)
1. a kind of preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating, it is characterised in that comprise the following steps：
Surface preparation：Semi-finished product surface of Nd-Fe-B permanent magnet is cleaned, 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 gun to described
The surface of Nd-Fe-B permanent magnet carries out activation process；
Vacuum coating：Nd-Fe-B permanent magnet after activation is moved to the vacuum coating area of vacuum coating equipment, at≤100 DEG C, adopted
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.
2. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1, it is characterised in that：The combination
The thickness of layer is 10nm-1000nm, and the thickness of the inner protective layer is 1 μm -10 μm, and the thickness of the transition zone is 10nm-
1000nm, the thickness of the external protection is 0.3 μm -6 μm.
3. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1 or 2, it is characterised in that：It is described
One or more of the material of binder course in Al, Cr, Ti or stainless steel.
4. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1 or 2, it is characterised in that：It is described
One or more of the material of inner protective layer in Sn, Zn, Cu, Al, Si-Al, Zn-Al or Sn-Zn.
5. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1 or 2, it is characterised in that：It is described
The material of transition zone is selected from Sn, Zn, Al, Si-Al, Zn-Al, Sn-Zn, SnO2, ZnO or Al2O3In one or more.
6. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 1 or 2, it is characterised in that：It is described
The material of external protection is selected from Al2O3、AlN、Cr2O3、TiO2、SiO2、Si3N4, one or more in TiN or CrN.
7. 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 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 fluid and cleans；Take out after cleaning, rinsed using deionized water；Take out, be placed in supersonic cleaning machine after rinsing
It is cleaned by ultrasonic；Taken out after ultrasonic cleaning, secondary rinsing is carried out using deionized water.
8. the preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating according to claim 7, it is characterised in that the cleaning
The composition of liquid is：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.
9. 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 in the ion activation area is 0.05Pa-3Pa, and the power of the ion gun is 3kW-7kW, living
The change time is 0.5min-3min.
10. a kind of surface has the Nd-Fe-B permanent magnet of anti-corrosion insulation coating, it is characterised in that：The anti-corrosion insulation coating uses
Preparation method as described in claim any one of 1-9 prepares.
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| 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 |
| 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 |
| US20230008985A1 (en) * | 2019-12-24 | 2023-01-12 | Deepinfar Ocean Technology Inc. | Permanent magnet rotor structure for 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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