CN106128744A - A kind of organic coating of Sintered NdFeB magnet surface temporary protection and preparation method thereof - Google Patents
A kind of organic coating of Sintered NdFeB magnet surface temporary protection and preparation method thereof Download PDFInfo
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- CN106128744A CN106128744A CN201610680263.0A CN201610680263A CN106128744A CN 106128744 A CN106128744 A CN 106128744A CN 201610680263 A CN201610680263 A CN 201610680263A CN 106128744 A CN106128744 A CN 106128744A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/026—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
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- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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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
- 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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/103—Anti-corrosive paints containing metal dust containing Al
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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
- 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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
Abstract
nullThe invention discloses organic coating of a kind of Sintered NdFeB magnet surface temporary protection and preparation method thereof，Use anode metal nano-particle (Al、Zn etc.) complex method to preparation silylation organic protection thin film be modified，The compound porosity that can significantly reduce thin film of nano-particle，Improve the uniform of magnet surface silylation organic protection thin film、Concordance，Simultaneously，Composite anode metal nano aluminium powder in silylation organic protection thin film、Nano zinc powder，Lost efficacy the initial stage at overcoat，Due to nano aluminum、The electro-chemical activity of zinc is apparently higher than the electrochemical potentials of NdFeB matrix，Therefore，Can be that matrix provides anode loss protection under electrochemical corrosion environment，Can continue to provide corrosion protection for magnet，Improve magnet surface silane film corrosion resisting property and mechanical property further，And the surface temporary anticorrosion organic coating finally obtaining excellent combination property.
Description
Technical field
The present invention relates to magnetic material surfacecti proteon field, the surface being specifically related to a kind of Sintered NdFeB magnet is temporary
The preparation of the organic coating of protection.
Background technology
Sintered NdFeB (NdFeB) magnet, since nineteen eighty-three comes out, has been widely used in the magnetic property of its excellence
The numerous areas such as electronics, motor, automobile, electric power, medical apparatus and instruments, instrument and meter, Aero-Space.But, by powder metallurgical technique
The Sintered NdFeB magnet of preparation has heterogeneous structure, and the electro-chemical activity of intergranular Nd-rich phase is high, causes magnet internal each
Between Xiang, potential difference is relatively big, in electrochemical environment, is easily generated galvanic corrosion, thus causes Sintered NdFeB magnet corrosion resisting property
Extreme difference, the serious further expansion limiting magnet applications field.It is commercially used for improving sintered NdFeB magnet at present corrosion proof
Method mainly has two kinds: one to be to add alloying element method；Two is to add protection painting/coating in magnet surface.But, add alloy
Element method is with the magnetic property sacrificing magnet as cost, adds cost prepared by magnet simultaneously, and the corrosion resisting property of magnet carries
High is limited in scope.Therefore, mode current industrial being typically employed in magnet surface interpolation protective coating improves the resistance to of magnet
Corrosive nature.
Protection painting/coating is by hindering contacting with each other between corrosive medium and matrix to slow down the corrosion of magnet, when
Front Sintered NdFeB magnet manufacturing carries out the mode of corrosion protection and mainly includes phosphatization, plating, chemical plating, negative electrode magnet
Electrophoresis, spraying, physical vapour deposition (PVD) etc..And use magnet applications field at electric motor of automobile, due to the later stage assemble during, need by
Magnet glue seals, thus, it is only required to magnet is carried out temporary protection, to avoid magnet to send out in later stage packaging and transportation
Raw corrosion.Current Sintered NdFeB magnet temporary protection technique is mainly phosphating process.But, after bonderizing, great Liang Han
The discharge of phosphorus waste water is easily generated serious environmental pollution, causes the cost of later stage three-protection design to increase.
Summary of the invention
The present invention uses temporary organic protection technique that sintered Nd-Fe-B permanent magnet is carried out surface process.Wherein, γ-
Aminopropyl triethoxysilane, phenyltrimethoxysila,e are that a class is containing silica-based hybrid thing, its basic molecular formula
For: R'(CH2)nSi(OR)3.Wherein OR is hydrolyzable group, and R' is organo-functional group.By its SiOH base after silane hydrolyzate
The shrink reaction of group and the MeOH group (Me represents metal) of metal surface and quick adsorption are in metal surface.On the one hand silane exists
Forming Si-O-Me covalent bond on metal interface, therefore the combination between silane and metal is the most firm；On the other hand, surplus
By the polycondensation reaction between SiOH group, in metal surface, formation has Si-O-Si tridimensional network to remaining silane molecule
Silane film.But, porosity height, bad dispersibility, mechanical property and the corrosion resisting property of the simple silane film of magnet surface deposition are poor.
Therefore, in order to improve the problem of above-mentioned existence, nano-particle (nano aluminum granule, Nano-Zinc granule etc.) can be used to mix
Silane film to be prepared is modified by miscellaneous mode, and chemical property and extremely strong affinity that nano-particle is prominent can be obvious
Reduce the porosity of silane film, improve the dispersibility of magnet surface silane film, it is thus achieved that the silane film uniform, concordance is good.And
Doping metals nanometer aluminium powder, nano zinc powder in organosilan film, can increase substantially the mechanical property of film layer, meanwhile, anti-
Sheath lost efficacy the initial stage, due to aluminum, zinc electro-chemical activity apparently higher than the electrochemical potentials of NdFeB matrix, therefore, in electrochemistry
Can be that matrix provides anode loss protection under corrosive environment, it is possible to continue as magnet and corrosion protection is provided, improve magnet surface silicon
Alkane film corrosion resisting property, it is thus achieved that the surface temporary anticorrosion organic coating of excellent combination property.
The present invention is directed to the deficiency that prior art exists, it is provided that a kind of for Sintered NdFeB magnet surface temporary protection
The preparation method of organic coating, it is intended to be effectively improved mechanical property and the corrosion resisting property of the simple silane film in neodymium-iron-boron surface
The defect of difference, provides a kind of preparation cost low, simple to operation and environmentally friendly for neodymium-iron-boron surface temporary protection
Surface protection process.
For solving the problems referred to above, the technical solution used in the present invention is as follows:
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface temporary protection, it is characterised in that under including
State step:
(1) Sintered NdFeB magnet is removed the pre-treatment of magnet surface oxide-film；
(2) preparation silylation Organic Alcohol solution；
(3) in above-mentioned silylation Organic Alcohol solution, anode metal nano-particle is added；
(4) above-mentioned Sintered NdFeB magnet is immersed in the silicon of the doping anode metal nano-particle of preparation in step (3)
Alkyl Organic Alcohol solution carries out surface-coated process；
(5) magnet after coating step (4) carries out cured.
The pretreatment process in step (1) carried out Sintered NdFeB magnet comprises the steps:
It is the HNO of 25% with mass fraction3Solution carries out pickling processes to Sintered NdFeB magnet, and the time is 5-10s；
Magnet after pickling processes is carried out ultrasonic cleaning；
By the HNO that magnet mass fraction is 1-3% after ultrasonic cleaning3Sintered NdFeB magnet is soaked by solution
Bubble, the time is 10-20s；
Magnet after soaking carries out second time ultrasonic cleaning；
Being immersed in alkaline solution by magnet after second time ultrasonic cleaning and soak, the time is 3-5min；
Then magnet alcohol washes, and carry out drying up process.
Further, described alkaline solution includes NaOH or KOH.
Further, described silylation Organic Alcohol solution is by γ-aminopropyl triethoxysilane, phenyl trimethoxy
Silane, ethylene glycol, deionized water, acetic acid, dehydrated alcohol are formulated.Preferably, γ-aminopropyl triethoxysilane, phenyl
Trimethoxy silane, deionized water, dehydrated alcohol, ethylene glycol configuration proportion successively is (1-3): (1-2): (0.8-1.2): (3-
5):(3-6).Further, described anode metal nano-particle is nano aluminum granule or Nano-Zinc granule, and its particle size range exists
Between 50-100nm.
Further, step (3) specifically includes following steps:
By silylation Organic Alcohol solution stirring more than 12 hours, solution is made uniformly to mix；
In above-mentioned silylation Organic Alcohol solution, add anode metal nano-particle and be stirred, every 1 hour, Ying Jiang
Solution utilizes ultrasonator to carry out ultrasonic vibration 15min, and mixing time is 5-10 hour.
Further, in step (4), Sintered NdFeB magnet uses immersion mode to be dip coating manner, and the time is 2-6min.
Further, described cured is to be placed in magnet in drying baker to solidify, and temperature is 100-180 DEG C, time
Between be 50-90min.
Further, described anode metal nano-particle processes through ultrasonic disperse, adding of described anode metal nano-particle
Dosage is 10-50g/L.
A kind of Sintered NdFeB magnet surface organic coating utilizing above-mentioned preparation method to prepare.
Compared with prior art, beneficial effects of the present invention is embodied in:
The preparation method of a kind of organic coating for Sintered NdFeB magnet surface temporary protection of the present invention, uses sun
The silylation organic protection thin film of preparation is modified by pole metal nanoparticle complex method, and the compound of nano-particle can show
Write the porosity reducing thin film, improve uniform, the concordance of magnet surface silylation organic protection thin film.And have at silylation
Composite anode metal nano aluminium powder, nano zinc powder in machine protection film, can increase substantially the mechanical property of film layer, improves film layer
Intensity and hardness.
Meanwhile, magnet is being carried out in plated film pretreatment process, using high concentration salpeter solution to remove the oxygen of magnet surface
Changing film, now, the corrosion of magnet is homogeneous corrosion, can reach the purpose stripping magnet surface oxide-film rapidly and uniformly.Then
With the nitric acid of low concentration, magnet being carried out pickling again, now, the corrosion of magnet is selective corrosion, can be by magnet surface intergranular
Rich neodymium the most preferentially erode.At the inefficacy initial stage of magnet surface anode nanometer Particles dispersed silylation organic protection thin film, by
Electro-chemical activity in aluminum, zinc is higher than the electro-chemical activity of neodymium iron boron magnetic body, therefore, the nano zinc powder in laminated film or aluminium powder
Can be that magnet provides anode loss protection under electrochemical corrosion environment, improve magnet surface silylation organic protection further thin
The corrosion resisting property of film, it is thus achieved that the temporary corrosion-inhibiting coating in surface of excellent combination property.The present invention is Sintered NdFeB magnet surface
Temporary protection provides the surface protection process that a kind of preparation cost is low, simple to operation and environmentally friendly.
Detailed description of the invention
Following embodiment is to further illustrate using as the explaination to the technology of the present invention content for present invention, but
The flesh and blood of the present invention is not limited in described in following embodiment, those of ordinary skill in the art can and should know appoint
What simple change based on true spirit or replacement all should belong to protection domain of the presently claimed invention.
Embodiment 1
The present embodiment prepares the organic coating of a kind of temporary protection as follows on Sintered NdFeB magnet surface:
(1) Sintered NdFeB magnet is carried out pre-treatment:
First, it is the HNO of 25% with mass fraction3Solution carries out pickling processes, pickling time to Sintered NdFeB magnet
5s, carries out ultrasonic cleaning by the magnet after pickling processes, by the HNO that magnet mass fraction is 3% after ultrasonic cleaning3Solution
Soaking Sintered NdFeB magnet, the time is 10s, and the magnet after soaking carries out second time ultrasonic cleaning, will second time
Magnet after ultrasonic cleaning immerses and soaks 3min in NaOH solution；Finally, from NaOH solution, take out magnet alcohol washes, then
Dry up stand-by with cold wind；
(2) preparation silylation Organic Alcohol solution:
To γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol five
Person prepares for 1:1:0.8:3:3 by volume, uses the pH value of vinegar acid-conditioning solution, described silylation Organic Alcohol solution
Stirring 12h, each component mix homogeneously in making solution；
(3) the silylation Organic Alcohol solution of configuration adds in step (2) anode metal aluminum nanoparticles:
First, in step (2), the silylation Organic Alcohol solution of configuration adds 10g/L anode metal aluminum nanoparticles, right
Silylation Organic Alcohol solution after doping anode metal nano-particle is stirred, and the time is 5h, meanwhile, every 1h, and should be by molten
Liquid is positioned over ultrasonic vibration 15min on ultrasonator；
(4) Sintered NdFeB magnet after processing step (1), using dip coating manner to be immersed in, step (3) prepares mixes
The silylation Organic Alcohol solution of miscellaneous nano-particle carries out surface-coated process:
Sintered NdFeB magnet after step (1) being processed, uses dip coating manner to be immersed in the doping that step (3) prepares and receives
Being coated in the solution of silane of rice grain processing, magnet time of immersion is 2min；
(5) magnet after step (4) coating is carried out cured:
Magnet after coating step (4) carries out cured and includes: the magnet after coating is placed in drying baker solidification,
Its solidification temperature is: 100 DEG C, and hardening time is: 50min.The present embodiment gained sample named sample 1A.
Comparative example 1
For contrasting, only prepare simple silylation organic protection thin film as follows on Sintered NdFeB magnet surface
The sample of (undoped p anode metal aluminum nanoparticles), named sample 1B: by technique identical for sample 1A carry out step (1),
Step (2), the sintered NdFeB magnet after then step (1) being processed, use dip coating manner to be immersed in the silicon that step (2) is prepared
Being coated in alkyl Organic Alcohol solution processing, magnet time of immersion is 2min.Finally, the magnet after coating is placed in drying baker
Middle solidification, its solidification temperature is: 100 DEG C, and hardening time is: 50min.
Gained sample 1A compares with sample 1B, and coating pencil hardness test data are shown in Table 1, coating salt spray test data (salt
The condition of mist test is: proof box temperature is 36 DEG C, and brine strength is 5% (volume ratio), uses the test method of spraying continuously)
It is shown in Table 2.
Can be seen that the coating hardness of sample 1A and salt fog resistance corrosive power are all shown compared with sample 1B from table 1, table 2
The raising write, illustrates that the technological measure of composite nanometer particle can be obviously improved single silylation in silylation Organic Alcohol solution
The adhesion of organic protection thin film, mechanical property and the problem of anticorrosion ability difference, thus significantly improve Sintered NdFeB magnet
Corrosion Protection.
Table 1 coating pencil hardness test data
| Sample | Pencil hardness |
| Sample 1B | 1H |
| Sample 1A | 2H |
Table 2 coating salt spray test data
| Sample | Sample 1B | Sample 1A |
| Salt spray test | 8h surface oxidisation | 14h surface is unchanged |
Embodiment 2
The present embodiment prepares the organic coating of a kind of temporary protection as follows on Sintered NdFeB magnet surface:
(1) Sintered NdFeB magnet is carried out pre-treatment:
It is the HNO of 25% with mass fraction3Solution carries out pickling processes, pickling time 8s to Sintered NdFeB magnet, incites somebody to action
Magnet after pickling processes carries out ultrasonic cleaning, is the HNO of 2% by the magnet mass fraction after ultrasonic cleaning3Solution is to burning
Knot neodymium iron boron magnetic body soaks, and the time is 15s, and the magnet after soaking carries out second time ultrasonic cleaning, by ultrasonic for second time
Magnet after cleaning immerses and soaks 4min in NaOH solution；Finally, from NaOH solution, take out magnet alcohol washes, then with cold
Wind is done stand-by；
(2) preparation silylation Organic Alcohol solution:
To γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol five
Person prepares for 2:1.5:1:4:4 by volume, uses the pH value of vinegar acid-conditioning solution, described silylation Organic Alcohol solution
Stirring 15h, each component mix homogeneously in making solution；
(3) the silylation Organic Alcohol solution of configuration adds in step (2) anode metal aluminum nanoparticles:
First, in step (2), the silylation Organic Alcohol solution of configuration adds 30g/L anode metal aluminum nanoparticles, right
Silylation Organic Alcohol solution after doping anode metal nano-particle is stirred, and the time is 8h, meanwhile, every 1h, and should be by molten
Liquid is positioned over ultrasonic vibration 15min on ultrasonator；
(4) Sintered NdFeB magnet after processing step (1), using dip coating manner to be immersed in, step (3) prepares mixes
The silylation Organic Alcohol solution of miscellaneous nano-particle carries out surface-coated process:
Sintered NdFeB magnet after step (1) being processed, uses dip coating manner to be immersed in the doping that step (3) prepares and receives
Being coated in the solution of silane of rice grain processing, magnet time of immersion is 4min；
(5) magnet after step (4) coating is carried out cured:
Magnet after coating step (4) carries out cured and includes: the magnet after coating is placed in drying baker solidification,
Its solidification temperature is: 150 DEG C, and hardening time is: 70min.The present embodiment gained sample named sample 2A.
Comparative example 2
For contrasting, only prepare simple silylation organic protection thin film as follows on Sintered NdFeB magnet surface
The sample of (undoped p anode metal aluminum nanoparticles), named sample 2B: by technique identical for sample 2A carry out step (1),
Step (2), the Sintered NdFeB magnet after then step (1) being processed, use dip coating manner to be immersed in the silicon that step (2) is prepared
Being coated in alkyl Organic Alcohol solution processing, magnet time of immersion is 4min.Finally, the magnet after coating is placed in drying baker
Middle solidification, its solidification temperature is: 150 DEG C, and hardening time is: 70min.
Gained sample 2A compares with sample 2B, and its coating pencil hardness test data are shown in Table 3, coating salt spray test data
(condition of salt spray test is: proof box temperature is 36 DEG C, and brine strength is 5% (volume ratio), uses the test side of spraying continuously
Formula) it is shown in Table 4.
Can be seen that the coating pencil hardness of sample 2A and salt fog resistance corrosive power all obtain compared with sample 2B from table 3, table 4
To significantly improving, illustrate that the technological measure of composite nanometer particle can be obviously improved single silicon in silylation Organic Alcohol solution
The adhesion of alkyl organic protection thin film, mechanical property and the problem of anticorrosion ability difference, thus significantly improve sintered NdFeB
The Corrosion Protection of magnet.
Table 3 coating pencil hardness test data
| Sample | Pencil hardness |
| Sample 2B | 1H |
| Sample 2A | 2H |
Table 4 coating salt spray test data
| Sample | Sample 2B | Sample 2A |
| Salt spray test | 10h surface oxidisation | 16h surface is unchanged |
Embodiment 3
(1) Sintered NdFeB magnet is carried out pre-treatment:
First, it is the HNO of 25% with mass fraction3Solution carries out pickling processes, pickling time to Sintered NdFeB magnet
10s, carries out ultrasonic cleaning by the magnet after pickling processes, by the HNO that magnet mass fraction is 1% after ultrasonic cleaning3Molten
Sintered NdFeB magnet is soaked by liquid, and the time is 20s, and the magnet after soaking carries out second time ultrasonic cleaning, by second
Magnet after secondary ultrasonic cleaning immerses and soaks 5min in NaOH solution；Finally, from NaOH solution, take out magnet alcohol washes,
Dry up stand-by again with cold wind；
(2) preparation silylation Organic Alcohol solution:
To γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol four
Person prepares for 3:2:1.2:5:6 by volume, uses the pH value of vinegar acid-conditioning solution, described silylation Organic Alcohol solution
Stirring 20h, each component mix homogeneously in making solution；
(3) the silylation Organic Alcohol solution of configuration adds in step (2) anode metal aluminum nanoparticles:
First, in step (2), the silylation Organic Alcohol solution of configuration adds 50g/L anode metal aluminum nanoparticles, right
Silylation Organic Alcohol solution after doping anode metal nano-particle is stirred, and the time is 10h, meanwhile, every 1h, and should be by molten
Liquid is positioned over ultrasonic vibration 15min on ultrasonator；
(4) Sintered NdFeB magnet after processing step (1), using dip coating manner to be immersed in, step (3) prepares mixes
The silylation Organic Alcohol solution of miscellaneous nano-particle carries out surface-coated process:
Sintered NdFeB magnet after step (1) being processed, uses dip coating manner to be immersed in the doping that step (3) prepares and receives
Being coated in the solution of silane of rice grain processing, magnet time of immersion is 6min；
(5) magnet after step (4) coating is carried out cured:
Magnet after coating step (4) carries out cured and includes: the magnet after coating is placed in drying baker solidification,
Its solidification temperature is: 180 DEG C, and hardening time is: 90min.The present embodiment gained sample named sample 3A.
Comparative example 2
For contrasting, only prepare simple silylation organic protection thin film as follows on Sintered NdFeB magnet surface
The sample of (undoped p anode metal aluminum nanoparticles), named sample 3B: by technique identical for sample 3A carry out step (1),
Step (2), the Sintered NdFeB magnet after then step (1) being processed, use dip coating manner to be immersed in the silicon that step (2) is prepared
Being coated in alkyl Organic Alcohol solution processing, magnet time of immersion is 6min.Finally, the magnet after coating is placed in drying baker
Middle solidification, its solidification temperature is: 180 DEG C, and hardening time is: 90min.
Gained sample 3A compares with sample 3B, and its coating pencil hardness test data are shown in Table 5, coating salt spray test data
(condition of salt spray test is: proof box temperature is 36 DEG C, and brine strength is 5% (volume ratio), uses the test side of spraying continuously
Formula) it is shown in Table 6.
Can be seen that the coating pencil hardness of sample 3A and salt fog resistance corrosive power all obtain compared with sample 3B from table 5, table 6
To significantly improving, illustrate that the technological measure of composite nanometer particle can be obviously improved single silicon in silylation Organic Alcohol solution
The adhesion of alkyl organic protection thin film, mechanical property and the problem of anticorrosion ability difference, thus significantly improve sintered NdFeB
The Corrosion Protection of magnet.
Table 5 coating pencil hardness test data
Table 6 coating salt spray test data
| Sample | Sample 3B | Sample 3A |
| Salt spray test | 12h surface oxidisation | 20h surface is unchanged |
Claims (11)
1. the preparation method of the organic coating of a Sintered NdFeB magnet surface temporary protection, it is characterised in that include following
Step:
(1) Sintered NdFeB magnet is removed the pre-treatment of magnet surface oxide-film；
(2) preparation silylation Organic Alcohol solution；
(3) in above-mentioned silylation Organic Alcohol solution, anode metal nano-particle is added；
(4) above-mentioned Sintered NdFeB magnet is immersed in the silylation of the doping anode metal nano-particle of preparation in step (3)
Organic Alcohol solution carries out surface-coated process；
(5) magnet after coating step (4) carries out cured.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that, the pretreatment process carrying out Sintered NdFeB magnet comprises the steps:
With the HNO that mass fraction is 25 %3Solution carries out pickling processes to Sintered NdFeB magnet, and the time is 5-10 s；
Magnet after pickling processes is carried out ultrasonic cleaning；
By the HNO that magnet mass fraction is 1-3 % after ultrasonic cleaning3Sintered NdFeB magnet is soaked by solution, time
Between be 10-20 s；
Magnet after soaking carries out second time ultrasonic cleaning；
Being immersed in alkaline solution by magnet after second time ultrasonic cleaning and soak, the time is 3-5 min；
Then magnet alcohol washes, and carry out drying up process.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 2 temporary protection,
It is characterized in that, described alkaline solution includes NaOH or KOH.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that, described silylation Organic Alcohol solution is by γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, second
Glycol, deionized water, acetic acid, dehydrated alcohol are formulated.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that, γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol depend on
Secondary configuration proportion is (1-3): (1-2): (0.8-1.2): (3-5): (3-6).
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that, described anode metal nano-particle is nano aluminum granule or Nano-Zinc granule, and its particle size range is at 50-100nm
Between.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that, step (3) specifically includes following steps:
By silylation Organic Alcohol solution stirring more than 12 hours, solution is made uniformly to mix；
In above-mentioned silylation Organic Alcohol solution, add anode metal nano-particle and be stirred, every 1 hour, should be by solution
Utilizing ultrasonator to carry out ultrasonic vibration 15 min, mixing time is 5-10 hour.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that: in step (4), Sintered NdFeB magnet uses immersion mode to be dip coating manner, and the time is 2-6 min.
The preparation method of the organic coating of a kind of Sintered NdFeB magnet surface the most as claimed in claim 1 temporary protection,
It is characterized in that, described cured is to be placed in magnet in drying baker to solidify, and temperature is 100-180 DEG C, and the time is
50-90 min。
The preparation side of the organic coating of a kind of Sintered NdFeB magnet surface temporary protection the most as claimed in claims 6 or 7
Method, it is characterised in that described anode metal nano-particle processes through ultrasonic disperse, the addition of described anode metal nano-particle
It is 10-50 g/L.
The organic painting in Sintered NdFeB magnet surface prepared by 11. 1 kinds of preparation methoies as described in any one of claim 1-10
Layer.
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