CN113275224B - Surface corrosion protection method for neodymium iron boron permanent magnet - Google Patents
Surface corrosion protection method for neodymium iron boron permanent magnet Download PDFInfo
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- CN113275224B CN113275224B CN202110470906.XA CN202110470906A CN113275224B CN 113275224 B CN113275224 B CN 113275224B CN 202110470906 A CN202110470906 A CN 202110470906A CN 113275224 B CN113275224 B CN 113275224B
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- iron powder
- iron boron
- neodymium iron
- permanent magnet
- carbonyl iron
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 118
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000005260 corrosion Methods 0.000 title claims abstract description 28
- 230000007797 corrosion Effects 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000011248 coating agent Substances 0.000 claims abstract description 31
- 238000000576 coating method Methods 0.000 claims abstract description 31
- 230000003075 superhydrophobic effect Effects 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001868 water Inorganic materials 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 92
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 60
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 60
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 59
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 45
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 37
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 37
- 239000011259 mixed solution Substances 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000001723 curing Methods 0.000 claims description 24
- SVMGVNXXUVNGRK-UHFFFAOYSA-N oxomethylideneiron Chemical class O=C=[Fe] SVMGVNXXUVNGRK-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000003760 magnetic stirring Methods 0.000 claims description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 10
- 239000003607 modifier Substances 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 3
- PMQIWLWDLURJOE-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F PMQIWLWDLURJOE-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 238000005507 spraying Methods 0.000 description 27
- 229910021642 ultra pure water Inorganic materials 0.000 description 11
- 239000012498 ultrapure water Substances 0.000 description 11
- 210000004081 cilia Anatomy 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 238000005536 corrosion prevention Methods 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229920001410 Microfiber Polymers 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
Abstract
The invention relates to the field of surface protection of neodymium iron boron permanent magnets, and discloses a surface corrosion protection method of a neodymium iron boron permanent magnet, aiming at solving the problem that the existing surface protection method aiming at neodymium iron boron is long and complex. The treated surface of the neodymium iron boron permanent magnet is provided with the super-hydrophobic coating with the micro-cilium structure, the super-hydrophobic coating can effectively isolate water and oxygen, the neodymium iron boron permanent magnet has excellent corrosion resistance, the micro-cilium structure has excellent toughness, the neodymium iron boron permanent magnet is endowed with excellent wear resistance and mechanical stability, and the neodymium iron boron permanent magnet is suitable for neodymium iron boron magnets with different sizes and different shapes, is simple and convenient to operate and has no pollution.
Description
Technical Field
The invention relates to the field of neodymium iron boron permanent magnets, in particular to a surface corrosion protection method of a neodymium iron boron permanent magnet.
Background
The neodymium iron boron permanent magnet has extremely high magnetic energy product, coercive force and energy density, and is widely applied to modern industry due to excellent magnetic performance. The neodymium element in the neodymium iron boron permanent magnet is used as one of metals with higher chemical activity, and the neodymium iron boron permanent magnet is very active in property, so that the neodymium iron boron permanent magnet is extremely easy to corrode; in addition, in the multiphase structure of ndfeb, the potential difference between the phases is large, so that it is very easy to react and corrode due to contact with water or oxygen in a high-temperature environment or a damp-heat environment. The existing surface protection method for the neodymium iron boron is long and complex, and a surface corrosion protection method for the neodymium iron boron permanent magnet with simple steps and good corrosion prevention effect is needed.
For example, an "anti-corrosion surface coating material for a neodymium iron boron permanent magnet" disclosed in the chinese patent document, whose publication number is CN202463036U, includes a surface coating layer for a neodymium iron boron permanent magnet material, which is an electroplated Ni layer, a chemical plated Ni layer, an electroplated Cu layer, a chemical plated Ni layer, and an electroplated Ni layer in this order from inside to outside. The method needs to plate multiple layers of films, the time for forming a surface microstructure is long, the process is complex, the early step of preparing various electroplating solutions is very complicated, and in addition, the method also has the problems of serious environmental pollution, high requirements on the size of a workpiece and the like.
For another example, a "method for corrosion prevention treatment of surface of neodymium iron boron magnet" disclosed in chinese patent document, whose publication number is CN108329724A, includes the following steps: pretreating the neodymium iron boron magnet; step two: carrying out phosphating treatment on the pretreated neodymium iron boron magnet; step three: spraying the phosphated neodymium iron boron magnet; step four: pre-curing the sprayed neodymium iron boron magnet at the temperature of 90-130 ℃ for 10-30 min; step five: and curing the neodymium iron boron magnet after curing at the temperature of 160-200 ℃ for 30-45 min. According to the method, before the neodymium iron boron permanent magnet is sprayed, the neodymium iron boron permanent magnet needs to be subjected to pretreatment and phosphorization, and the curing process after spraying also needs to be finished in two steps, so that the steps are complicated; moreover, the coating components used for spraying comprise 8 substances, the components are complex, 3 substances need to be ground for 5 hours, 4 substances need to be put into a reaction kettle for pre-reaction for 5 hours, and the preparation time is long.
Disclosure of Invention
The invention provides a surface corrosion protection method for a neodymium iron boron permanent magnet, which is simple and convenient to operate and rapid to prepare, and aims to overcome the problems of complex steps and long reaction time in the prior art. According to the invention, the super-hydrophobic coating is sprayed on the surface of the neodymium iron boron permanent magnet, and the micro-cilium structure is constructed on the surface of the neodymium iron boron permanent magnet and solidified by utilizing the intrinsic magnetism of the neodymium iron boron permanent magnet, so that the super-hydrophobic coating has good corrosion resistance, and is suitable for surface protection of neodymium iron boron permanent magnets of different sizes and different shapes.
In order to achieve the purpose, the invention adopts the following technical scheme:
a surface corrosion protection method of a neodymium iron boron permanent magnet comprises the steps of spraying a super-hydrophobic coating on the surface of the neodymium iron boron permanent magnet, forming a micro-cilium structure on the surface of the neodymium iron boron by the super-hydrophobic coating under the action of a magnetic field, and then placing the neodymium iron boron permanent magnet in an oven for curing; the neodymium iron boron magnet is very easily corroded by the reaction because of contacting with water or oxygen, and the super hydrophobic coating can completely cut off the contact of neodymium iron boron magnet and water, oxygen, produces anticorrosive effect to the neodymium iron boron magnet to surface structure can influence the infiltration nature on surface to a certain extent, and the hydrophobic performance of super hydrophobic coating can further be promoted to little cilium structure.
Preferably, the super-hydrophobic coating is a modified carbonyl iron powder-PDMS mixed solution, and the preparation method comprises the following steps: a. dispersing carbonyl iron powder into an ethanol water solution, and heating, stirring and reacting the carbonyl iron powder with a silane modifier;
b. centrifuging the solution after reaction, and drying the precipitate to obtain modified carbonyl iron powder;
c. stirring and reacting the modified carbonyl iron powder, the PDMS and the curing agent in a solvent to obtain a modified carbonyl iron powder-PDMS mixed solution.
Carbonyl iron powder is magnetic, can adhere to on neodymium iron boron magnet surface and do not influence neodymium iron boron magnet magnetism, mix spraying with PDMS after the carbonyl iron powder is modified and make its solidification form super hydrophobic coating on neodymium iron boron magnet surface, can promote neodymium iron boron magnet's corrosion resistance and toughness, through neodymium iron boron magnet self magnetism, the carbonyl iron powder forms little cilium structure at neodymium iron boron magnet, and this structure can further strengthen anticorrosion and abrasionproof loss effect.
Preferably, the reaction conditions of step a are heating to 60-80 ℃, the magnetic stirring speed is 300-550rpm, and the reaction time is 5-7 h.
Preferably, the volume ratio of the absolute ethanol to the water in the ethanol water solution in the step a is 1:3-2: 1; the mass ratio of the carbonyl iron powder to the silane modifier is 20:1-10: 1.
The mass ratio of carbonyl iron powder to silane modifier can affect the yield of modified carbonyl iron powder, and the ratio of ethanol to water in the ethanol aqueous solution can affect the solubility of the silane modifier, thereby affecting the yield of modified carbonyl iron powder.
Preferably, the silane modifier in step a is heptadecafluorodecyltriethoxysilane.
The silane modifier can enable the surface of the carbonyl iron powder to generate silicon hydroxyl, and then the silicon hydroxyl reacts with a subsequent siloxane reagent to reduce the surface energy of the coating.
Preferably, the centrifugation condition of the step b is 5000-9000rpm, the centrifugation time is 5-10min, the drying condition is 50-70 ℃, and the drying time is 2-3 h.
Under the drying condition, the centrifuged precipitate can be dried until the water content is 2-8%.
Preferably, the ratio of the solvent in step c: PDMS: curing agent: the mass ratio of the modified carbonyl iron powder is 400:20:6:5-200:10:3: 5.
The property of PDMS makes the surface micro cilium structure formed have certain toughness, which makes the micro cilium structure of the coating not easy to be damaged, and can greatly increase the wear resistance and mechanical stability of the coating.
Preferably, the volume ratio of the absolute ethanol to the water in the ethanol water solution in the step a is 1:2-2:1, and the solvent in the step c: PDMS: curing agent: the mass ratio of the modified carbonyl iron powder is 400:20:6:5-600:30:9: 10.
When the ratio of ethanol to water is 1:2-2:1, the ratio of PDMS: when the mass ratio of the modified carbonyl iron powder is 3:1-4:1, the prepared super-hydrophobic coating has good micro-cilium structural morphology and hydrophobic effect.
Preferably, in the step c, the solvent is hexane or acetone or cyclohexanone, and the curing agent is Sylgard 184.
In order to fully dissolve the PDMS and the curing agent and uniformly disperse the PDMS and the curing agent, the solvent is selected from hexane, acetone or cyclohexanone, and the curing agent is used for maintaining the micro-cilia structure formed by the coating.
Preferably, the curing temperature is 35-60 ℃, and the curing time is longer than 2 h.
In the invention, PDMS and curing agent need to be heated and cured, and in order to prevent the neodymium iron boron magnet from demagnetizing, a low-temperature curing process is adopted.
Therefore, the invention has the following beneficial effects: (1) the surface contact between water and oxygen and the surface of the neodymium iron boron permanent magnet can be effectively isolated, so that the treated neodymium iron boron permanent magnet has excellent corrosion resistance, the application range of the neodymium iron boron permanent magnet can be greatly expanded, and the service life and the performance of the neodymium iron boron permanent magnet are obviously prolonged; (2) the magnetism of the carbonyl iron powder enables the coating to directly form a micro-cilium structure on the surface of the neodymium iron boron permanent magnet without being attached to other templates, and the adhesive force between the coating and the neodymium iron boron permanent magnet is enhanced; (3) the micro-fiber structure has good toughness, and endows the neodymium iron boron permanent magnet with excellent wear resistance and mechanical stability; (4) the method is suitable for batch surface treatment of neodymium iron boron magnets of different sizes and shapes, and is simple and convenient to operate and free of pollution.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
Fig. 2 is a surface SEM image of the neodymium iron boron magnet prepared in example 1.
Detailed Description
The invention is further described with reference to the accompanying drawings and specific embodiments.
Example 1
The preparation steps are shown in figure 1:
(1) preparing a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:2, and dispersing carbonyl iron powder in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 2
(1) Preparing a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:2, and dispersing carbonyl iron powder in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: uniformly stirring the modified carbonyl iron powder with a mass ratio of 200:10:3:5 on a magnetic stirrer at a speed of 150rpm for 10min to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and placing the solution in spraying equipment;
(5) taking a piece of neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 3
(1) Preparing a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:2, and dispersing carbonyl iron powder in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: uniformly stirring the modified carbonyl iron powder with a mass ratio of 400:20:6:5 on a magnetic stirrer at a speed of 150rpm for 10min to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and placing the solution in spraying equipment;
(5) taking a neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 4
(1) Dispersing carbonyl iron powder into absolute ethyl alcohol: the volume ratio of the ultrapure water is 2: 1;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a piece of neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 5
(1) Dispersing carbonyl iron powder into absolute ethyl alcohol: the volume ratio of the ultrapure water is 1: 1;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a piece of neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 6
(1) Dispersing carbonyl iron powder into absolute ethyl alcohol: the volume ratio of the ultrapure water is 1: 3;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of that of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution at 9000rpm for 5min by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 7
(1) Ultrapure water was used as the carbonyl iron powder dispersion;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 8
(1) Preparing a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:1, and dispersing carbonyl iron powder in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 10% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a piece of neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 9
(1) Preparing a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:1, and dispersing carbonyl iron powder in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 3% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution at 9000rpm for 5min by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 35 ℃.
Example 10
(1) Preparing a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:1, and dispersing carbonyl iron powder in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS, modified carbonyl iron powder and Sylgard184 were added to hexane: PDMS: sylgard 184: the mass ratio of the modified carbonyl iron powder is 600:30:9:10, the modified carbonyl iron powder is uniformly stirred for 10min on a magnetic stirrer at the speed of 150rpm to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, and the modified carbonyl iron powder-PDMS mixed solution is placed in spraying equipment;
(5) taking a neodymium iron boron magnet, controlling the distance between the nozzle and the neodymium iron boron magnet to be about 5cm, and spraying the mixed solution on the surface of the neodymium iron boron magnet;
(6) the magnet was placed in an oven to cure for 6h at 60 ℃.
Comparative example 1
(1) The dispersing agent is a solution with the volume ratio of anhydrous ethanol to ultrapure water being 1:1, and carbonyl iron powder is dispersed in the solution;
(2) heating the solution to 80 ℃, adding FAS-17 with the mass of 5% of the carbonyl iron powder under the condition of magnetic stirring at 550rpm, and continuously covering and stirring for 7 hours;
(3) centrifuging the reacted solution for 5min at 9000rpm by a centrifuge, placing the solution in a 50 ℃ oven, and drying for 3h to obtain modified carbonyl iron powder;
(4) PDMS and modified carbonyl iron powder were added to hexane, hexane: PDMS: the mass ratio of the modified carbonyl iron powder is 60:3:1, the modified carbonyl iron powder is uniformly stirred on a magnetic stirrer at the speed of 150rpm for 10min to obtain a uniformly mixed modified carbonyl iron powder-PDMS mixed solution, the mixed solution is placed in spraying equipment, the mixed solution is sprayed on the surface of neodymium iron boron, and then the magnet is placed in an oven to be cured for 6h at the temperature of 35 ℃.
Comparative example 2 is a neodymium iron boron magnet without spray protection of the superhydrophobic coating.
The surface contact angle detection is carried out on the neodymium iron boron magnet sprayed with the super-hydrophobic coating obtained in the examples 1-10 and the comparative example 1 respectively, and the detection steps are as follows:
a. putting the sample into an objective table of a contact angle tension measuring instrument, and adjusting the focal length to ensure that the image is clear;
b. 2.0 mul of water is pressed out by a micro-syringe;
c. lifting the object stage, and lowering the object stage to the original position after the surface of the sample contacts the liquid drops;
d. images of the droplets on the sample surface were taken and the results were analyzed.
The results are shown in table 1:
TABLE 1 surface contact angle of NdFeB magnets
| Item | Contact angle |
| Example 1 | 161.1° |
| Example 2 | 151.7° |
| Example 3 | 153.5° |
| Example 4 | 157.3° |
| Example 5 | 166.1° |
| Example 6 | 150.6° |
| Example 7 | 78.1° |
| Example 8 | 165.8° |
| Example 9 | 128.7° |
| Example 10 | 159.0° |
| Comparative example 1 | 142.8° |
| Comparative example 2 | 52.7° |
When the stable contact angle of the surface is more than 150 degrees and the rolling angle is less than 5 degrees, the surface is considered to be completely free of water, the surface waterproof coating has a good waterproof effect as shown in the table 1, and the hydrophobic effect is optimal when the mass ratio of the PDMS to the carbonyl iron powder is 3: 1; the ratio of ethanol to water in the dispersing agent can influence the solubility of the silane modifier and further influence the yield of the modified carbonyl iron powder, the effect is better when the ratio of the ethanol to the water is 1:3-2:1, and the effect is best when the ratio of the ethanol to the water is 1: 1.
In order to further judge the corrosion prevention effect of the super-hydrophobic coating, the corrosion current of the neodymium iron boron magnet obtained in example 1 and comparative example 2 is detected by using an electrochemical workstation, and the detection steps are as follows:
A. wrapping the rest surfaces of the neodymium iron boron magnet, only exposing one surface coated with the coating, and connecting the neodymium iron boron magnet with an electric wire;
B. detecting the corrosion current of the neodymium iron boron magnet by using a three-electrode system, wherein the neodymium iron boron magnet is used as a working electrode, a reference electrode is a calomel electrode, and an auxiliary electrode is a platinum electrode;
C. connecting the three electrodes with an electrochemical workstation, and then immersing the three electrodes into electrolyte, wherein the electrolyte is 3.5% of NaCl solution;
D. setting the corrosion voltage range to-0.3V-1.3V, scanning the neodymium iron boron magnet, recording the current magnitude in the process, and calculating the corrosion current density.
Example 1 the corrosion current density was-5.372X 10 -6 A·cm -2 And the corrosion current density of the neodymium iron boron magnet which is not protected by the super-hydrophobic coating spraying is-4.385 multiplied by 10 -7 A·cm -2 The corrosion resistance of the embodiment 1 is improved by one order of magnitude compared with the comparison 2, so that the super-hydrophobic coating prepared by the invention has good corrosion resistance to the neodymium iron boron magnet.
The appearance of the neodymium iron boron surface coating obtained in example 1 is observed by using SEM, and the result is shown in fig. 2, the superhydrophobic coating of the present invention forms a micro-cilia structure on the surface of the neodymium iron boron magnet, and the structure can further enhance the corrosion prevention and wear prevention effects. PDMS and carbonyl iron powder proportion and curing temperature all can influence little cilia structure, and when not consolidating the agent, modified carbonyl iron powder can appear lodging destruction little cilia structure for little cilia structure can't be fine and close formation in neodymium iron boron magnet surface, reduces corrosion resisting property.
The neodymium iron boron magnets obtained in examples 1, 2, 3, 4, 5 and 6 and comparative example 1 were subjected to a friction wear test, which specifically includes the following steps:
a. placing the coated side of the neodymium iron boron magnet to be tested on 800-mesh abrasive paper downwards;
b. pressing a 100g weight on the NdFeB magnet, horizontally dragging the NdFeB magnet to generate friction, and horizontally moving the NdFeB magnet back and forth by 10cm to be regarded as 1 friction cycle;
c. the surface contact angles of the ndfeb magnets after 0, 50, 100, 200 and 500 rubbing cycles were measured, respectively.
The results are shown in table 2:
TABLE 2 contact angle data after frictional wear of NdFeB magnets
| Period of friction | 0 | 50 | 100 | 200 | 500 |
| Example 1 | 161.1° | 157.9° | 157.5° | 154.3° | 151.4° |
| Example 2 | 151.7° | 146.3° | 144.8° | 141.4° | 137.9° |
| Example 3 | 153.5° | 149.2° | 147.6° | 144.8° | 142.9° |
| Example 4 | 157.3° | 155.4° | 153.7° | 151.2° | 148.6° |
| Example 5 | 166.1° | 163.1° | 162.9° | 161.6° | 157.3° |
| Example 6 | 150.6° | 148.7° | 147.1° | 144.6° | 140.8° |
| Comparative example 1 | 142.8° | 103.3° | 82.7° | 53.8° | 53.1° |
As can be seen from Table 2, as the number of times of friction increases, the cilia structure is abraded to some extent, the surface hydrophobic property of the NdFeB permanent magnet is reduced to some extent, the surface hydrophobic property of the comparative example 1 is reduced to the greatest extent, and when no curing agent is added during preparation, the cilia structure is extremely easy to damage; the extent of abrasion of the micro-ciliated structures of examples 1, 3, 4, 5 and 6 was relatively slow, and the decrease of the surface hydrophobic property was significantly lower than that of examples 2 and 1, thus it was found that when PDMS: the micro-cilium toughness is better when the mass ratio of the modified carbonyl iron powder is 4:1-3: 1; and after 500 friction cycles, the surface contact angle of the neodymium iron boron permanent magnet is still larger than 150 degrees in the embodiment 1 and the embodiment 5, the hydrophobicity is good, the toughness of the micro cilia is stronger, the distribution density is more reasonable, and the abrasion resistance is better.
Claims (8)
1. A surface corrosion protection method of a neodymium iron boron permanent magnet is characterized in that a super-hydrophobic coating is sprayed on the surface of the neodymium iron boron permanent magnet, and the super-hydrophobic coating forms a micro-cilium structure on the surface of the neodymium iron boron under the action of a magnetic field and then is placed in an oven for curing;
the super-hydrophobic coating is a modified carbonyl iron powder-PDMS mixed solution, and the preparation method comprises the following steps:
a. dispersing carbonyl iron powder into an ethanol water solution, and heating, stirring and reacting the carbonyl iron powder with a silane modifier;
b. centrifuging the solution after reaction, and drying the precipitate obtained in the centrifuging process to obtain modified carbonyl iron powder;
c. stirring and reacting modified carbonyl iron powder, PDMS and a curing agent in a solvent to obtain a modified carbonyl iron powder-PDMS mixed solution;
the solvent in the step c is as follows: PDMS: curing agent: the mass ratio of the modified carbonyl iron powder is 400:20:6:5-200:10:3: 5.
2. The method as claimed in claim 1, wherein the reaction conditions of step a are heating to 60-80 ℃, magnetic stirring speed of 300-.
3. The method for preventing corrosion of the surface of the neodymium iron boron permanent magnet according to claim 1 or 2, wherein the volume ratio of absolute ethyl alcohol to water in the ethyl alcohol water solution in the step a is 1:3-2: 1; the mass ratio of the carbonyl iron powder to the silane modifier is 20:1-10: 1.
4. The method for protecting surface corrosion of neodymium iron boron permanent magnet according to claim 1 or 2, wherein the silane modifier in step a is heptadecafluorodecyltriethoxysilane.
5. The method for protecting surface corrosion of neodymium iron boron permanent magnet according to claim 1, wherein the centrifugation condition of step b is 5000-9000rpm, the centrifugation time is 5-10min, the drying condition is 50-70 ℃, and the drying time is 2-3 h.
6. The surface corrosion protection method for the neodymium-iron-boron permanent magnet according to claim 1 or 2, wherein the volume ratio of absolute ethyl alcohol to water in the ethyl alcohol water solution in the step a is 1:2-2:1, and the solvent in the step c is as follows: PDMS: curing agent: the mass ratio of the modified carbonyl iron powder is 400:20:6:5-600:30:9: 10.
7. The method for protecting surface corrosion of NdFeB permanent magnet as claimed in claim 1 or 6, wherein in step c the solvent is hexane or acetone or cyclohexanone and the curing agent is Sylgard 184.
8. The method for protecting the surface of the neodymium-iron-boron permanent magnet from corrosion according to claim 1, wherein the curing temperature is 35-60 ℃, and the curing time is longer than 2 hours.
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Application publication date: 20210820 Assignee: Zhejiang Zhongke magnetic Co.,Ltd. Assignor: HANGZHOU DIANZI University Contract record no.: X2024330000005 Denomination of invention: A surface corrosion protection method for neodymium iron boron permanent magnets Granted publication date: 20220923 License type: Common License Record date: 20240108 |