CN106128744B - A kind of Sintered NdFeB magnet surface temporary protection organic coating and preparation method - Google Patents
A kind of Sintered NdFeB magnet surface temporary protection organic coating and preparation method Download PDFInfo
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- CN106128744B CN106128744B CN201610680263.0A CN201610680263A CN106128744B CN 106128744 B CN106128744 B CN 106128744B CN 201610680263 A CN201610680263 A CN 201610680263A CN 106128744 B CN106128744 B CN 106128744B
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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
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- 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
The invention discloses a kind of organic coatings and preparation method thereof of Sintered NdFeB magnet surface temporary protection, using anode metal nano particle (Al, Zn etc.) complex method is modified the silylation organic protection film of preparation, the compound porosity that can significantly reduce film of nano particle, improve the uniform of magnet surface silylation organic protection film, consistency, simultaneously, the composite anode metal nano aluminium powder in silylation organic protection film, nano zinc powder, it fails initial stage in protective layer, due to nano aluminum, the electro-chemical activity of zinc is apparently higher than the electrochemical potentials of NdFeB matrix, therefore, under electrochemical corrosion environment anode loss protection can be provided for matrix, it can continue to provide corrosion protection for magnet, further increase magnet surface silane film corrosion resisting property and mechanical property, and it finally obtains comprehensive The excellent temporary anti-corrosion organic coating in surface of energy.
Description
Technical field
The present invention relates to magnetic material surfacecti proteon fields, and in particular to a kind of surface of Sintered NdFeB magnet is temporary
The preparation of the organic coating of protection.
Background technique
Sintered NdFeB (NdFeB) magnet has been widely used in since nineteen eighty-three comes out with its excellent magnetic property
The numerous areas such as electronics, motor, automobile, electric power, medical instrument, instrument and meter, aerospace.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 each inside magnet
Potential difference is larger between phase, in electrochemical environment, is also easy to produce galvanic corrosion, to cause Sintered NdFeB magnet corrosion resisting property
It is very poor, the serious further expansion for limiting magnet applications field.It is corrosion proof that it is commercially used for raising sintered NdFeB magnet at present
There are mainly two types of methods: first is that addition alloying element method；Second is that adding protection painting/coating in magnet surface.But addition alloy
Element method is while to increase the cost of magnet preparation to sacrifice the magnetic property of magnet as cost, and the corrosion resisting property of magnet mentions
High is limited in scope.Therefore, the mode that magnet surface addition protective coating is typically employed in current industrial improves the resistance to of magnet
Corrosive nature.
Protection painting/coating be by hindering contacting with each other between corrosive medium and matrix to slow down the corrosion of magnet, when
The mode that preceding Sintered NdFeB magnet manufacturing carries out corrosion protection to magnet mainly includes phosphatization, plating, chemical plating, cathode
Electrophoresis, spraying, physical vapour deposition (PVD) etc..And in electric motor of automobile magnet applications field, due in later period assembling process, need by
Magnet is sealed with glue, thus, it is only required to carry out temporary protection to magnet, is sent out in later period packaging and transportational process to avoid magnet
Raw corrosion.Current Sintered NdFeB magnet temporary protection technique is mainly phosphating process.However, after phosphorating treatment, great Liang Han
The discharge of phosphorus waste water is also easy to produce serious environmental pollution, causes the increased costs of later period three-protection design.
Summary of the invention
The present invention is surface-treated sintered Nd-Fe-B permanent magnet using temporary organic protection technique.Wherein, γ-
Aminopropyl triethoxysilane, phenyltrimethoxysila,e are a kind of hybrid object containing silicon substrate, basic molecular formula
Are as follows: R'(CH2) nSi (OR) 3.Wherein OR is hydrolyzable group, and R' is organo-functional group.Pass through its SiOH base after silane hydrolyzate
Group reacted with the shrink of the MeOH group of metal surface (Me expression metal) and quick adsorption in metal surface.One side silane exists
Si-O-Me covalent bond is formed on metal interface, therefore the combination between silane and metal is very firm；On the other hand, it remains
Remaining silane molecule, which is formed by the polycondensation reaction between SiOH group in metal surface, has Si-O-Si tridimensional network
Silane film.But the porosity height of the simple silane film of magnet surface deposition, bad dispersibility, mechanical property and corrosion resisting property are poor.
Therefore, in order to improve above-mentioned problem, nano particle (nanometer alumina particles, Nano-Zinc particle etc.) can be used and mix
Miscellaneous mode is modified silane film to be prepared, and nano particle chemical property outstanding and extremely strong affinity can be obvious
The porosity of silane film is reduced, the dispersibility of magnet surface silane film is improved, obtains silane film uniform, that consistency 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 fails initial stage, since the electro-chemical activity of aluminium, zinc is apparently higher than the electrochemical potentials of NdFeB matrix, in electrochemistry
Anode loss protection can be provided for matrix under corrosive environment, can continue to provide corrosion protection for magnet, improve magnet surface silicon
Alkane film corrosion resisting property obtains the temporary anti-corrosion organic coating in surface of excellent combination property.
The present invention is in view of the deficienciess of the prior art, provide a kind of for Sintered NdFeB magnet surface temporary protection
Organic coating preparation method, it is intended to be effectively improved the mechanical property and corrosion resisting property of the simple silane film in neodymium iron boron magnetic body surface
The defect of difference, it is low, simple to operation and environmentally friendly to provide a kind of preparation cost for neodymium iron boron magnetic body surface temporary protection
Surface protection process.
To solve the above problems, 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 including under
State step:
(1) pre-treatment of magnet surface oxidation film is removed to Sintered NdFeB magnet；
(2) the organic alcoholic solution of silylation is prepared；
(3) anode metal nano particle is added in the organic alcoholic solution of above-mentioned silylation；
(4) above-mentioned Sintered NdFeB magnet is immersed in the silicon for the doping anode metal nano particle prepared in step (3)
Surface coating processing is carried out in the organic alcoholic solution of alkyl；
(5) curing process is carried out to the magnet after step (4) coating.
The pretreatment process carried out in step (1) to Sintered NdFeB magnet includes the following steps:
Pickling processes, time 5-10s are carried out to Sintered NdFeB magnet with the HNO3 solution that mass fraction is 25%；
Magnet after pickling processes is cleaned by ultrasonic；
The HNO3 solution that magnet after ultrasonic cleaning is 1-3% with mass fraction soaks Sintered NdFeB magnet
Bubble, time 10-20s；
Magnet after immersion is carried out second to be cleaned by ultrasonic；
Magnet after second is cleaned by ultrasonic, which immerses in alkaline solution, to be impregnated, time 3-5min；
Then magnet alcohol washes, and carry out drying processing.
Further, the alkaline solution includes NaOH or KOH.
Further, the organic alcoholic solution of the silylation is by γ-aminopropyl triethoxysilane, phenyl trimethoxy
Silane, ethylene glycol, deionized water, acetic acid, dehydrated alcohol are formulated.Preferably, γ-aminopropyl triethoxysilane, phenyl
Successively configuration proportion is (1-3): (1-2): (0.8-1.2): (3- for trimethoxy silane, deionized water, dehydrated alcohol, ethylene glycol
5):(3-6).Further, the anode metal nano particle is that nanometer alumina particles or Nano-Zinc particle, particle size range exist
Between 50-100nm.
Further, step (3) specifically includes the following steps:
The organic alcoholic solution of silylation is stirred 12 hours or more, mix solution uniformly；
It adds and anode metal nano particle and is stirred in the organic alcoholic solution of above-mentioned silylation, every 1 hour, Ying Jiang
Solution carries out ultrasonic vibration 15min using ultrasonator, and mixing time is 5-10 hours.
Further, Sintered NdFeB magnet uses immersion mode for dip coating manner in step (4), time 2-6min.
Further, the curing process is that magnet is placed in drying box to solidify, and temperature is 100-180 DEG C, when
Between be 50-90min.
Further, the anode metal nano particle is handled through ultrasonic disperse, and the anode metal nano particle adds
Dosage is 10-50g/L.
A kind of Sintered NdFeB magnet surface organic coating prepared using above-mentioned preparation method.
Compared with prior art, the beneficial effects of the present invention are embodied in:
A kind of preparation method of the organic coating for Sintered NdFeB magnet surface temporary protection of the present invention, using sun
Pole metal nanoparticle complex method is modified the silylation organic protection film of preparation, and the compound of nano particle can be shown
The porosity for reducing film is write, uniform, the consistency of magnet surface silylation organic protection film are improved.And have in silylation
Composite anode metal nano aluminium powder, nano zinc powder in machine protection film can increase substantially the mechanical property of film layer, improve film layer
Intensity and hardness.
Meanwhile being carried out in plated film pretreatment process to magnet, using the oxygen of high concentration salpeter solution removal magnet surface
Change film, at this point, the corrosion of magnet is homogeneous corrosion, can reach the purpose for rapidly and uniformly stripping magnet surface oxidation film.Then
Pickling is carried out to magnet with the nitric acid of low concentration again, at this point, the corrosion of magnet is selective corrosion, it can be by magnet surface intergranular
Nd-rich phase preferentially erode.At the failure initial stage of magnet surface anode nanometer Particles dispersed silylation organic protection film, by
It is higher than the electro-chemical activity of neodymium iron boron magnetic body, therefore, nano zinc powder or aluminium powder in laminated film in the electro-chemical activity of aluminium, zinc
Anode loss protection can be provided for magnet under electrochemical corrosion environment, it is thin to further increase magnet surface silylation organic protection
The corrosion resisting property of film obtains 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.
Specific embodiment
Following embodiments are further explanations for the content of present invention using as the explaination to the technology of the present invention content, but
Substantive content of the invention is not limited in described in following embodiments, those skilled in the art can with and should know appoint
What simple change or replacement based on true spirit should belong to protection scope of the presently claimed invention.
Embodiment 1
The present embodiment prepares a kind of organic coating of temporary protection on Sintered NdFeB magnet surface as follows:
(1) pre-treatment is carried out to Sintered NdFeB magnet:
Firstly, carrying out pickling processes, pickling time to Sintered NdFeB magnet with the HNO3 solution that mass fraction is 25%
Magnet after pickling processes is cleaned by ultrasonic by 5s, the HNO3 solution for being 3% by the magnet mass fraction after ultrasonic cleaning
Sintered NdFeB magnet is impregnated, time 10s, the magnet after immersion is carried out second and is cleaned by ultrasonic, it will be second
Magnet after ultrasonic cleaning, which immerses in NaOH solution, impregnates 3min；Finally, magnet alcohol washes are taken out from NaOH solution, then
It is stand-by with cold wind drying；
(2) the organic alcoholic solution of silylation is prepared:
To γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol five
Person is that 1:1:0.8:3:3 is prepared by volume, using the pH value of vinegar acid-conditioning solution, the organic alcoholic solution of the silylation
12h is stirred, each component in solution is uniformly mixed；
(3) anode metal aluminum nanoparticles are added in the organic alcoholic solution of silylation configured in step (2):
Firstly, the organic alcoholic solution of the silylation configured in step (2) adds 10g/L anode metal aluminum nanoparticles, it is right
The organic alcoholic solution of silylation after doping anode metal nano particle is stirred, time 5h, meanwhile, it, should will be molten every 1h
Liquid is placed in ultrasonic vibration 15min on ultrasonator；
(4) to step (1) treated Sintered NdFeB magnet, mixing for step (3) preparation is immersed in using dip coating manner
Surface coating processing is carried out in the organic alcoholic solution of the silylation of miscellaneous nano particle:
By step (1) treated Sintered NdFeB magnet, received using the doping that dip coating manner is immersed in step (3) preparation
Coating processing is carried out in the solution of silane of rice grain, magnet time of immersion is 2min；
(5) curing process is carried out to the magnet after step (4) coating:
Carrying out curing process to the magnet after step (4) coating includes: that the magnet after coating is placed in drying box to solidify,
Its solidification temperature are as follows: 100 DEG C, curing time are as follows: 50min.Sample obtained by the present embodiment is named as sample 1A.
Comparative example 1
To compare, simple silylation organic protection film is only prepared on Sintered NdFeB magnet surface as follows
The sample of (undoped with anode metal aluminum nanoparticles), is named as sample 1B: by identical technique progress step (1) of sample 1A,
Step (2) is immersed in the silicon of step (2) preparation using dip coating manner then by step (1) treated sintered NdFeB magnet
Coating processing is carried out in the organic alcoholic solution of alkyl, magnet time of immersion is 2min.Finally, being placed in drying box to the magnet after coating
Middle solidification, solidification temperature are as follows: 100 DEG C, curing time are as follows: 50min.
Gained sample 1A is compared 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 are as follows: chamber temperature is 36 DEG C, and brine strength is 5% (volume ratio), using continuously spraying test method)
It is shown in Table 2.
From table 1, table 2 it can be seen that the coating hardness and salt fog resistance corrosive power of sample 1A are shown compared with sample 1B
The raising of work illustrates that the technological measure of the composite nanometer particle in the organic alcoholic solution of silylation can be obviously improved single silylation
The problem of the binding force of organic protection film, mechanical property and anticorrosion ability difference, to significantly improve Sintered NdFeB magnet
Corrosion Protection.
1 coating pencil hardness test data of table
| Sample | Pencil hardness |
| Sample 1B | 1H |
| Sample 1A | 2H |
2 coating salt spray test data of table
| Sample | Sample 1B | Sample 1A |
| Salt spray test | 8h surface oxidisation | The surface 14h is unchanged |
Embodiment 2
The present embodiment prepares a kind of organic coating of temporary protection on Sintered NdFeB magnet surface as follows:
(1) pre-treatment is carried out to Sintered NdFeB magnet:
The HNO3 solution for being 25% with mass fraction carries out pickling processes to Sintered NdFeB magnet, and pickling time 8s will
Magnet after pickling processes is cleaned by ultrasonic, by the magnet mass fraction after ultrasonic cleaning be 2% HNO3 solution to burning
Knot neodymium iron boron magnetic body is impregnated, time 15s, and the magnet after immersion is carried out second and is cleaned by ultrasonic, will second of ultrasound
Magnet after cleaning, which immerses in NaOH solution, impregnates 4min；Finally, taking out magnet alcohol washes from NaOH solution, then with cold
Wind is dry stand-by；
(2) the organic alcoholic solution of silylation is prepared:
To γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol five
Person is that 2:1.5:1:4:4 is prepared by volume, using the pH value of vinegar acid-conditioning solution, the organic alcoholic solution of the silylation
15h is stirred, each component in solution is uniformly mixed；
(3) anode metal aluminum nanoparticles are added in the organic alcoholic solution of silylation configured in step (2):
Firstly, the organic alcoholic solution of the silylation configured in step (2) adds 30g/L anode metal aluminum nanoparticles, it is right
The organic alcoholic solution of silylation after doping anode metal nano particle is stirred, time 8h, meanwhile, it, should will be molten every 1h
Liquid is placed in ultrasonic vibration 15min on ultrasonator；
(4) to step (1) treated Sintered NdFeB magnet, mixing for step (3) preparation is immersed in using dip coating manner
Surface coating processing is carried out in the organic alcoholic solution of the silylation of miscellaneous nano particle:
By step (1) treated Sintered NdFeB magnet, received using the doping that dip coating manner is immersed in step (3) preparation
Coating processing is carried out in the solution of silane of rice grain, magnet time of immersion is 4min；
(5) curing process is carried out to the magnet after step (4) coating:
Carrying out curing process to the magnet after step (4) coating includes: that the magnet after coating is placed in drying box to solidify,
Its solidification temperature are as follows: 150 DEG C, curing time are as follows: 70min.Sample obtained by the present embodiment is named as sample 2A.
Comparative example 2
To compare, simple silylation organic protection film is only prepared on Sintered NdFeB magnet surface as follows
The sample of (undoped with anode metal aluminum nanoparticles), is named as sample 2B: by identical technique progress step (1) of sample 2A,
Step (2) is immersed in the silicon of step (2) preparation using dip coating manner then by step (1) treated Sintered NdFeB magnet
Coating processing is carried out in the organic alcoholic solution of alkyl, magnet time of immersion is 4min.Finally, being placed in drying box to the magnet after coating
Middle solidification, solidification temperature are as follows: 150 DEG C, curing time are as follows: 70min.
Gained sample 2A is compared with sample 2B, and coating pencil hardness test data are shown in Table 3, coating salt spray test data
(the condition of salt spray test are as follows: chamber temperature is 36 DEG C, and brine strength is 5% (volume ratio), using continuously spraying test side
Formula) it is shown in Table 4.
From table 3, table 4 it can be seen that the coating pencil hardness and salt fog resistance corrosive power of sample 2A obtain compared with sample 2B
It is improved to significant, illustrates that the technological measure of the composite nanometer particle in the organic alcoholic solution of silylation can be obviously improved single silicon
The problem of the binding force of alkyl organic protection film, mechanical property and anticorrosion ability difference, to significantly improve sintered NdFeB
The Corrosion Protection of magnet.
3 coating pencil hardness test data of table
| Sample | Pencil hardness |
| Sample 2B | 1H |
| Sample 2A | 2H |
4 coating salt spray test data of table
| Sample | Sample 2B | Sample 2A |
| Salt spray test | 10h surface oxidisation | The surface 16h is unchanged |
Embodiment 3
(1) pre-treatment is carried out to Sintered NdFeB magnet:
Firstly, carrying out pickling processes, pickling time to Sintered NdFeB magnet with the HNO3 solution that mass fraction is 25%
Magnet after pickling processes is cleaned by ultrasonic by 10s, and the HNO3 for being 1% by the magnet mass fraction after ultrasonic cleaning is molten
Liquid impregnates Sintered NdFeB magnet, time 20s, and the magnet after immersion is carried out second and is cleaned by ultrasonic, by second
Magnet after secondary ultrasonic cleaning, which immerses in NaOH solution, impregnates 5min；Finally, magnet alcohol washes are taken out from NaOH solution,
It is dried up again with cold wind stand-by；
(2) the organic alcoholic solution of silylation is prepared:
To γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol four
Person is that 3:2:1.2:5:6 is prepared by volume, using the pH value of vinegar acid-conditioning solution, the organic alcoholic solution of the silylation
20h is stirred, each component in solution is uniformly mixed；
(3) anode metal aluminum nanoparticles are added in the organic alcoholic solution of silylation configured in step (2):
Firstly, the organic alcoholic solution of the silylation configured in step (2) adds 50g/L anode metal aluminum nanoparticles, it is right
The organic alcoholic solution of silylation after doping anode metal nano particle is stirred, time 10h, meanwhile, it, should will be molten every 1h
Liquid is placed in ultrasonic vibration 15min on ultrasonator；
(4) to step (1) treated Sintered NdFeB magnet, mixing for step (3) preparation is immersed in using dip coating manner
Surface coating processing is carried out in the organic alcoholic solution of the silylation of miscellaneous nano particle:
By step (1) treated Sintered NdFeB magnet, received using the doping that dip coating manner is immersed in step (3) preparation
Coating processing is carried out in the solution of silane of rice grain, magnet time of immersion is 6min；
(5) curing process is carried out to the magnet after step (4) coating:
Carrying out curing process to the magnet after step (4) coating includes: that the magnet after coating is placed in drying box to solidify,
Its solidification temperature are as follows: 180 DEG C, curing time are as follows: 90min.Sample obtained by the present embodiment is named as sample 3A.
Comparative example 2
To compare, simple silylation organic protection film is only prepared on Sintered NdFeB magnet surface as follows
The sample of (undoped with anode metal aluminum nanoparticles), is named as sample 3B: by identical technique progress step (1) of sample 3A,
Step (2) is immersed in the silicon of step (2) preparation using dip coating manner then by step (1) treated Sintered NdFeB magnet
Coating processing is carried out in the organic alcoholic solution of alkyl, magnet time of immersion is 6min.Finally, being placed in drying box to the magnet after coating
Middle solidification, solidification temperature are as follows: 180 DEG C, curing time are as follows: 90min.
Gained sample 3A is compared with sample 3B, and coating pencil hardness test data are shown in Table 5, coating salt spray test data
(the condition of salt spray test are as follows: chamber temperature is 36 DEG C, and brine strength is 5% (volume ratio), using continuously spraying test side
Formula) it is shown in Table 6.
From table 5, table 6 it can be seen that the coating pencil hardness and salt fog resistance corrosive power of sample 3A obtain compared with sample 3B
It is improved to significant, illustrates that the technological measure of the composite nanometer particle in the organic alcoholic solution of silylation can be obviously improved single silicon
The problem of the binding force of alkyl organic protection film, mechanical property and anticorrosion ability difference, to significantly improve sintered NdFeB
The Corrosion Protection of magnet.
5 coating pencil hardness test data of table
6 coating salt spray test data of table
| Sample | Sample 3B | Sample 3A |
| Salt spray test | 12h surface oxidisation | The surface 20h is unchanged |
Claims (10)
1. a kind of preparation method of Sintered NdFeB magnet surface temporary protection organic coating, it is characterised in that: including following
Step:
(1) pre-treatment of magnet surface oxidation film is removed to Sintered NdFeB magnet, the pre-treatment is first with quality point
The HNO of number 25%3Solution pickling, then the HNO for being 1-3 % with mass fraction3Solution impregnates；
(2) the organic alcoholic solution of silylation is prepared, the organic alcoholic solution of silylation is by γ-aminopropyl triethoxysilane, benzene
Base trimethoxy silane, ethylene glycol, deionized water, acetic acid, dehydrated alcohol are formulated；
(3) anode metal nano particle is added in the organic alcoholic solution of above-mentioned silylation；
(4) above-mentioned Sintered NdFeB magnet is immersed in the silylation for the doping anode metal nano particle prepared in step (3)
Surface coating processing is carried out in organic alcoholic solution；
(5) curing process is carried out to the magnet after step (4) coating, solidification temperature is 100-180 DEG C, time 50-90
Min forms the organosilan film of doping anode metal nano particle on Sintered NdFeB magnet surface.
2. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as described in claim 1, feature
Be: the pretreatment process carried out to Sintered NdFeB magnet includes the following steps:
The HNO for being 25 % with mass fraction3Solution carries out pickling processes to Sintered NdFeB magnet, and the time is 5-10 s；
Magnet after pickling processes is cleaned by ultrasonic；
The HNO for being 1-3 % with mass fraction by the magnet after ultrasonic cleaning3Solution impregnates Sintered NdFeB magnet, when
Between be 10-20 s；
Magnet after immersion is carried out second to be cleaned by ultrasonic；
Magnet after second is cleaned by ultrasonic, which immerses in alkaline solution, to be impregnated, and the time is 3-5 min；
Then magnet alcohol washes, and carry out drying processing.
3. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as claimed in claim 2, feature
Be: the alkaline solution includes NaOH or KOH.
4. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as described in claim 1, feature
It is, γ-aminopropyl triethoxysilane, phenyltrimethoxysila,e, deionized water, dehydrated alcohol, ethylene glycol are successively prepared
Ratio is (1-3): (1-2): (0.8-1.2): (3-5): (3-6).
5. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as described in claim 1, feature
Be: the anode metal nano particle is nanometer alumina particles or Nano-Zinc particle, and particle size range is between 50-100nm.
6. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as described in claim 1, feature
Be: step (3) specifically includes the following steps:
The organic alcoholic solution of silylation is stirred 12 hours or more, mix solution uniformly；
Anode metal nano particle is added in the organic alcoholic solution of above-mentioned silylation and is stirred, it, should be by solution every 1 hour
15 min of ultrasonic vibration is carried out using ultrasonator, mixing time is 5-10 hours.
7. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as described in claim 1, feature
Be: Sintered NdFeB magnet uses immersion mode for dip coating manner in step (4), time 2-6min.
8. the preparation method of Sintered NdFeB magnet surface temporary protection organic coating as described in claim 1, feature
Be: the curing process is that magnet is placed in drying box to solidify.
9. special such as the preparation method of Sintered NdFeB magnet surface temporary protection organic coating described in claim 5 or 6
Sign is: the anode metal nano particle is handled through ultrasonic disperse, and the anode metal nano particle additive amount is 10-
50g/L。
10. a kind of Sintered NdFeB magnet surface such as the described in any item preparation method preparations of claim 1-9 is temporary anti-
Protect organic coating.
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| CN111354561A (en) * | 2020-03-25 | 2020-06-30 | 余姚市宏伟磁材科技有限公司 | Neodymium iron boron surface treatment technology |
| CN114582618A (en) * | 2022-03-09 | 2022-06-03 | 合肥工业大学 | Nanoparticle-doped composite coating and preparation method and application thereof |
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