CN107739534A - A kind of alcohol radical inorganic composite coating and preparation method thereof - Google Patents
A kind of alcohol radical inorganic composite coating and preparation method thereof Download PDFInfo
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- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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Abstract
The invention provides a kind of alcohol radical inorganic composite coating and preparation method thereof, the alcohol radical inorganic composite coating is made up of inorganic sol and inorganic filler, wherein, inorganic sol includes Ludox, TiO 2 sol and alkoxy silane and the hydrolysate of titanate esters, and inorganic filler includes the one or more in aluminium powder, silver powder, alumina powder, oxide powder and zinc, titanium dioxide, graphite powder and silica flour.By alcohol radical inorganic composite coating prepared by the method for the present invention on the premise of ensureing that coating and basal body binding force, magnetic property are unaffected, the decay resistance of coating can be greatly improved, can apply to Nd-Fe-B magnetic material surfacecti proteon field.
Description
Technical field
The present invention relates to Nd-Fe-B magnetic material surfacecti proteon field, is applied more particularly, to a kind of alcohol radical inorganic compounding
Layer and preparation method thereof.
Background technology
Nd-Fe-B permanent magnet material is the third generation rare earth permanent-magnetic material after samarium cobalt rare earth permanent magnet, and there is high remanent magnetism, height to rectify
The advantages that stupid power and high energy product, electronic product, computer, instrument and meter, high-fidelity loudspeaker, vapour have been widely used in it
The various fields such as turner industry, Medical Devices, energy traffic, wind-power electricity generation and Aero-Space.China by rare earth resources advantage and
Production cost advantage, neodymium iron boron magnetic body industry is greatly developed, have become the first in the world big producer and consumption big country.
But because Nd-Fe-B materials chemistries activity is strong, be easily oxidized, corrosion-resistant, cause the reduction of its magnetic property.
And rich B phases, rich-Nd phase, the electrochemical potentials of Nd2Fe14B phases are different in sintered Nd-Fe-B permanent magnetic material, rich-Nd phase
Electrode potential than matrix Nd2Fe14B mutually it is more negative, large number of rich neodymium phase, is easily formed in damp and hot environment on crystal boundary
Corrode micro cell, constitute many big negative electrode (Nd2Fe14B) the micro cell group mutually formed with primary anode (Nd phases), so that rich
Nd phases are corroded first, and serious intercrystalline corrosion occurs, and cause material efflorescence, cause magnetic property drastically to decline.Therefore, typically all
Need to carry out coating treatment to neodymium iron boron magnetic body surface.
At present in Nd-Fe-B magnetic material surface treatment mainly based on plating and chemical plating, such as：Electroplated Ni layer, electricity
Plate the technologies such as Zn layers, combination electroplated Ni CuNi layers, Electroless Plating Ni layer, electrophoresis, the corrosion resisting properties of these coating is still within relatively low
Standard, can not meet the application under more adverse circumstances, but processing procedure is more strict and complicated, and at these surfaces
Reason technical process generally can all cause serious environmental pollution.
Therefore, have a kind of environmental protection to be developed, technique be simple, coating corrosion resistance can it is good, ensure coating and basal body binding force,
The impregnable Nd-Fe-B magnetic material surface coated treatment technology of magnetic property.
The content of the invention
For the surface protection techniques such as current plating, chemical plating exist it is seriously polluted and can not meet neodymium iron boron magnetic body compared with
The problems such as to be applied under rugged environment, it is inorganic to improve the corrosion proof alcohol radical of neodymium iron boron magnetic body it is an object of the invention to provide one kind
Coating and preparation method thereof.The present invention utilizes alcohol radical inorganic coating process for treating surface, and operating procedure is easy, and cost is cheap,
On the premise of ensureing that coating and basal body binding force, magnetic property are unaffected, the decay resistance of coating can be greatly improved, effectively
Solve the pollution problem of neodymium iron boron magnetic body surfacecti proteon and apply upper limitation, prevent plating, dirt of the chemical plating process to environment
Dye.
The invention provides a kind of alcohol radical inorganic composite coating, the alcohol radical inorganic composite coating is by inorganic sol and inorganic
Filler forms, wherein, the inorganic sol includes Ludox, TiO 2 sol and alkoxy silane and metatitanic acid ester hydrolysis
Product, the inorganic filler include one in aluminium powder, silver powder, alumina powder, oxide powder and zinc, titanium dioxide, graphite powder and silica flour
Kind is a variety of.
In above-mentioned alcohol radical inorganic composite coating, the institutional framework of the alcohol radical inorganic composite coating is crystalline state and amorphous state
Composite construction or crystalline state composite construction.
Present invention also offers a kind of method for preparing alcohol radical inorganic composite coating, comprise the following steps：
Ludox and TiO 2 sol are mixed；Titanate esters and aqueous hydrochloric acid solution are added, pH is adjusted, reaction, adds
Alkoxy silane and the first alcoholic solvent and ammoniacal liquor, reaction, obtain silicon titanium complex sol；By the silicon titanium complex sol and inorganic
Filler is added in the second alcoholic solvent, obtains alcohol radical inorganic compounding coating；And the alcohol radical inorganic compounding coating is sprayed
Apply, alcohol radical inorganic composite coating is prepared.
In the above-mentioned methods, the Ludox be by average grain diameter be 40~80nm silica ethanol, isopropanol,
The dispersion formed in one or more dispersion solvents in n-butanol and DAA；The TiO 2 sol is by putting down
Equal particle diameter is the 20~50nm nano titanium oxide one or more in ethanol, isopropanol, n-butanol and DAA point
Dissipate the dispersion formed in solvent.
In the above-mentioned methods, the mass fraction of the silica in the Ludox is 5%~10%, the titanium dioxide
The mass fraction of titanium dioxide in colloidal sol is 3%~5%.
In the above-mentioned methods, the titanate esters include one in purity titanium tetraethoxide, butyl titanate and tetraisopropyl titanate
Kind is a variety of；First alcoholic solvent and second alcoholic solvent include alcohol solvent, isopropanol solvent, n-butanol solvent respectively
With the one or more in DAA solvent.
In the above-mentioned methods, the inorganic filler includes aluminium powder, silver powder, alumina powder, oxide powder and zinc, titanium dioxide, graphite
One or more in powder and silica flour, the granularity of the inorganic filler is 100~2000 mesh.
In the above-mentioned methods, in addition to：Before the alcohol radical inorganic compounding coating is sprayed, first magnet is carried out
Chamfered, polishing derusting then is carried out with emery cloth, pickling processes are carried out to magnet with nitric acid afterwards, then it is ultrasonic with absolute ethyl alcohol
Cleaning, the magnet after ultrasonic cleaning is soaked in absolute ethyl alcohol.
In the above-mentioned methods, it is described the alcohol radical inorganic compounding coating is subjected to spraying to include：Using layering spraying method
Magnet surface after the pre-treatment is sprayed, and magnet surface first after the pre-treatment sprays one layer of subbing；Then exist
An aspect coating is sprayed on the subbing subbing, then carries out drying and processing.
In the above-mentioned methods, the subbing is made up of anticracking powder and the alcohol radical inorganic compounding coating, the surface layer
Coating is the alcohol radical inorganic compounding coating,
Wherein, the mass percent that the anticracking powder accounts for the gross mass of the subbing is 3%~5%.
In the above-mentioned methods, the drying and processing includes being pre-reacted to mem stage and the low-temperature sintering stage of reaction, institute successively
It is that the low-temperature sintering stage of reaction is using 150 using 80 DEG C~170 DEG C 10~30min of baking to state and be pre-reacted to mem stage
DEG C~250 DEG C of 30~90min of baking.
Compared with prior art, the beneficial effects of the present invention are：
The present invention carries out surfacecti proteon using alcohol radical inorganic composite coating to neodymium iron boron magnetic body, has that technique is simple, operation
It is convenient, cost is cheap, have on the premise of ensureing that the adhesion of coating and matrix, magnetic property are unaffected excellent corrosion-resistant
In more than 1000h corrosion does not occur for performance, resistance to neutral salt spray time；And the inorganic coating of the present invention is free of chromium, without toxic
Solvent, heavy metal free pollution, it can effectively solve the problem that the environmental pollution that neodymium iron boron magnetic body plating, chemical plating process of surface treatment are brought
Problem and the upper limitation of application.
Embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
The invention provides a kind of alcohol radical inorganic composite coating, the coating is by amorphous inorganic colloidal sol and crystalline inorganic filler
Composition, and the institutional framework of the alcohol radical inorganic composite coating is crystalline state and amorphous-state composite structures or crystalline state composite construction, can
Effectively prevent the coating surface from aoxidizing, increase the corrosion resistance of coating；Wherein, amorphous inorganic colloidal sol forms the basic knot of coating
Structure, in three-dimensional netted cross structure, main component is Ludox, nano-TiO2The water of colloidal sol and alkoxy silane and titanate esters
Solve product, can be combined closely with neodymium-iron-boron body interface, and crystalline inorganic filler mainly include aluminium powder, silver powder, alumina powder,
One or more in oxide powder and zinc, titanium dioxide, graphite powder and silica flour, it can be evenly distributed in amorphous inorganic colloidal sol,
And the use of inorganic filler can effectively improve coating corrosion resistance.
Present invention also offers a kind of method for preparing alcohol radical inorganic composite coating, this method is first with Ludox, nanometer
TiO2Colloidal sol, titanate esters, alkoxy silane, crystalline inorganic filler and alcoholic solvent are raw material, are existed using titanate esters, alkoxy silane
The hydrolytic-polymeric reaction occurred in alcoholic solvent prepares alcohol radical inorganic compounding coating；Then chamfering is carried out to neodymium iron boron magnetic body
The surface preparations such as processing, oil removing, derusting；Afterwards, alcohol radical inorganic compounding coating is sprayed to the neodymium iron boron magnetic body after surface treatment,
Alcohol radical inorganic composite coating is formed after drying processing again, thickness is about 15~20 μm.
Concretely comprise the following steps：
(1) in mass ratio 5:1~2:1 to take the Ludox that mass fraction is 5%~10% and mass fraction be 3%~5%
Nano-TiO2Colloidal sol, it is well mixed under 300~600r/min stir speed (S.S.)；
(2) it is 1 to be added in the colloidal sol for continuing to be well mixed to step (1) under stirring condition with Ludox mass ratio:2~1:
4 titanate esters, at the same add mass fraction be 4~6% aqueous hydrochloric acid solution be used as acidic catalyst, regulation system pH value be 2
~4,2h~5h is reacted at room temperature；Afterwards, it is 6 to add with titanate esters mass ratio:1~4:1 alkoxy silane (the second of methyl three
TMOS or tetraethoxysilane), and it is 8 to add with alkoxy silane mass ratio:1~3:1 the first alcoholic solvent, add simultaneously
Enter the ammoniacal liquor that mass fraction is 25%, it is 5 to make the mol ratio of ammoniacal liquor and element silicon:1~3:1, stirred at 50 DEG C~70 DEG C anti-
8h~10h is answered, prepares silicon titanium complex sol；
(3) under room temperature condition, in mass ratio 10:1~2:The 1 silicon titanium complex sol and crystalline inorganic for obtaining step (2)
Filler adds sand mill, while it is 8 to add with crystalline inorganic packing quality ratio:1~4:1 the second alcoholic solvent grinding 3h~5h,
So as to prepare alcohol radical inorganic compounding coating.
(4) alcohol radical inorganic compounding coating is sprayed, alcohol radical inorganic coating is prepared.
In the method, Ludox be by average grain diameter be 40~80nm silica in ethanol, isopropanol, n-butanol
Or the dispersion formed in one or more dispersion solvents in DAA；Nano-TiO2Colloidal sol be by average grain diameter be 20
~50nm anatase TiO2Formed in one or more dispersion solvents in ethanol, isopropanol, n-butanol or DAA
Dispersion.
In the method, titanate esters include purity titanium tetraethoxide, butyl titanate, one kind in tetraisopropyl titanate or more
Kind；First alcoholic solvent and the second alcoholic solvent include alcohol solvent, isopropanol solvent, n-butanol solvent or DAA solvent respectively
In one or more.
In the method, inorganic filler includes Al powder, silver powder, alumina powder, oxide powder and zinc, titanium dioxide, graphite powder and stone
One or more in English powder, the inorganic filler granularity are 100~2000 mesh.
This method also includes：Before alcohol radical inorganic compounding coating is sprayed, chamfering first is carried out to neodymium iron boron magnetic body
Processing, then carries out polishing derusting with emery cloth, carries out 10~15s of pickling processes to neodymium iron boron magnetic body with 1.5% dust technology afterwards,
It is cleaned by ultrasonic 2~3 times with absolute ethyl alcohol again, the neodymium iron boron magnetic body after ultrasonic cleaning is soaked into 5~10min in absolute ethyl alcohol,
Finally drying is handled.
In the method, alcohol radical inorganic compounding coating is carried out into spraying includes：Using layering spraying method after the pre-treatment
Neodymium iron boron magnetic body surface sprayed, magnet surface first after the pre-treatment sprays one layer of subbing, room temperature after spraying
Stand 5~10 minutes levellings；Then an aspect coating (that is, alcohol radical inorganic compounding coating) is sprayed, is stored at room temperature 5~10 minutes
Levelling, then carry out drying and processing.
In the method, subbing by anticracking powder (account for subbing gross mass mass percent be 3%~5%) and
Alcohol radical inorganic compounding coating obtains after stirring；Anticracking powder is nano-grade glass fibre or nanoscale nylon fiber powder, is selected
It nano-scale particle, can be easier to be scattered in coating, inorganic coating can be more equally distributed in after drying, heat treatment
On.
In the method, coated and dried processing includes being pre-reacted to mem stage and the low-temperature sintering stage of reaction successively, pre- anti-
It is using 80 DEG C~170 DEG C 10~30min of baking to answer text message, and the low-temperature sintering stage of reaction is using 150 DEG C~250 DEG C bakings
Roasting 30~90min.
Embodiment 1
(1) preparation of alcohol radical inorganic compounding coating：According to 3:1 mass ratio by mass fraction be 5% Ludox and matter
Measure the nano-TiO that fraction is 3%2Colloidal sol is well mixed under 500r/min stir speed (S.S.)s, is then added and Ludox mass ratio
For 1:2 titanate esters (mass ratio 1:1 purity titanium tetraethoxide and butyl titanate), use mass fraction for 5% hydrochloric acid water
Solution regulation system pH value is 4, reacts 5h at room temperature；In the case where continuing stirring condition, it is 5 to add with titanate esters mass ratio:1
Tetraethoxysilane, and add with tetraethoxysilane mass ratio be 5:1 alcoholic solvent (volume ratio 3:1 ethanol and two
Pyruvic alcohol), while the ammoniacal liquor that mass fraction is 25% is added, it is 3 to make the mol ratio of ammoniacal liquor and element silicon:1, stirred at 60 DEG C
8h is reacted, forms silicon titanium complex sol；Afterwards, according to 5:1:4 mass ratio is by above-mentioned silicon titanium complex sol, inorganic filler (matter
Amount is than being 1:1:1:2 Al powder, titanium dioxide, alumina powder and silica flour, granularity are 100 mesh) and alcoholic solvent (volume ratio 2:1
Ethanol and isopropanol) be added to sand mill, be ground 5h, prepare alcohol radical inorganic compounding coating.
(2) neodymium iron boron magnetic body surface preparation：Prepare neodymium iron boron magnetic body sample (50mm × 50mm × 5mm) first, it is first right
Neodymium iron boron magnetic body carries out chamfered, polishing derusting is carried out respectively with 150# sand paper and 600# sand paper, afterwards with 1.5% dust technology
Pickling processes 10s is carried out to neodymium iron boron magnetic body, then is cleaned by ultrasonic 3 times with absolute ethyl alcohol, by the neodymium iron boron magnetic body after ultrasonic cleaning
10min is soaked in absolute ethyl alcohol, is finally dried up.
(3) preparation of alcohol radical inorganic composite coating：Magnet surface first after the pre-treatment spray one layer of subbing (by
The alcohol radical inorganic compounding coating that with the addition of the anticracking powder of mass percent 3% is formed), 8 minutes levellings are stored at room temperature after spraying, then
An aspect coating (the alcohol radical inorganic compounding coating as prepared) is sprayed again, is stored at room temperature 8 minutes levellings, then carry out at drying
Reason, including 30min is toasted at a temperature of 100 DEG C, and toast 45min at a temperature of 180 DEG C.
Embodiment 2
(1) preparation of alcohol radical inorganic compounding coating：According to 2:1 mass ratio by mass fraction be 8% Ludox and matter
Measure the nano-TiO that fraction is 5%2Colloidal sol is well mixed under 600r/min stir speed (S.S.)s, is then added and Ludox mass ratio
For 1:2 titanate esters (mass ratio 1:1 purity titanium tetraethoxide and butyl titanate), use mass fraction for 4% hydrochloric acid water
Solution regulation system pH value is 2, reacts 3h at room temperature；In the case where continuing stirring condition, it is 5 to add with titanate esters mass ratio:1
Alkoxy silane (mass ratio 1:1 MTES and tetraethoxysilane), and addition and alkoxy silane
Mass ratio is 3:1 alcoholic solvent (volume ratio 3:1:1 ethanol, isopropanol and DAA), while add mass fraction and be
25% ammoniacal liquor, it is 5 to make the mol ratio of ammoniacal liquor and element silicon:1, the stirring reaction 10h at 50 DEG C, form silicon titanium complex sol；
Afterwards, according to 2:1:5 mass ratio is by above-mentioned silicon titanium complex sol, inorganic filler (mass ratio 1:2:1:1 silver powder, titanium white
Powder, alumina powder and silica flour, granularity are 1500 mesh) and alcoholic solvent (volume ratio 2:1 ethanol and isopropanol) it is added to sand milling
Machine, 3h is ground, prepares alcohol radical inorganic compounding coating.
(2) neodymium iron boron magnetic body surface preparation：Prepare neodymium iron boron magnetic body sample (50mm × 50mm × 5mm) first, it is first right
Neodymium iron boron magnetic body carries out chamfered, polishing derusting is carried out respectively with 150# sand paper and 600# sand paper, afterwards with 1.5% dust technology
Pickling processes 10s is carried out to neodymium iron boron magnetic body, then is cleaned by ultrasonic 3 times with absolute ethyl alcohol, by the neodymium iron boron magnetic body after ultrasonic cleaning
10min is soaked in absolute ethyl alcohol, is finally dried up.
(3) preparation of alcohol radical inorganic composite coating：One layer of bottom of neodymium iron boron magnetic body surface spraying first after the pre-treatment
Coating (is made up of) the alcohol radical inorganic compounding coating that with the addition of the anticracking powder of mass percent 5%, is stored at room temperature 5 minutes and is flowed after spraying
It is flat, an aspect coating (the alcohol radical inorganic compounding coating as prepared) is then sprayed again, is stored at room temperature 5 minutes levellings, then enter
Toasted at a temperature of row drying and processing, including 80 DEG C and toast 60min at a temperature of 15min, and 170 DEG C.
Embodiment 3
(1) preparation of alcohol radical inorganic compounding coating：According to 4:1 mass ratio by mass fraction be 10% Ludox and matter
Measure the nano-TiO that fraction is 5%2Colloidal sol is well mixed under 600r/min stir speed (S.S.)s, is then added and Ludox mass ratio
For 1:3 titanate esters (mass ratio 1:1 purity titanium tetraethoxide and tetraisopropyl titanate), use mass fraction for 5% hydrochloric acid
Aqueous solution regulation system pH value is 3, reacts 4h at room temperature；In the case where continuing stirring condition, add and be with titanate esters mass ratio
4:1 alkoxy silane (mass ratio 2:1 MTES and tetraethoxysilane), and add and silane quality
Than for 5:1 alcoholic solvent (volume ratio 2:1:1 ethanol, isopropanol and DAA), while mass fraction is added as 25%
Ammoniacal liquor, make the mol ratio of ammoniacal liquor and element silicon be 8:1, the stirring reaction 8h at 70 DEG C, form silicon titanium complex sol；Afterwards,
According to 8:1:8 mass ratio is by above-mentioned silicon titanium complex sol, inorganic filler (mass ratio 1:1:1:1:1 aluminium powder, titanium dioxide,
Alumina powder, oxide powder and zinc and silica flour, granularity are 1800 mesh) and alcoholic solvent (volume ratio 2:1:1 ethanol, isopropanol and just
Butanol) sand mill is added to, 5h is ground, prepares alcohol radical inorganic compounding coating.
(2) neodymium iron boron magnetic body surface preparation：Prepare neodymium iron boron magnetic body sample (80mm × 80mm × 5mm) first, it is first right
Neodymium iron boron magnetic body carries out chamfered, polishing derusting is carried out respectively with 150# sand paper and 600# sand paper, afterwards with 1.5% dust technology
Pickling processes 10s is carried out to neodymium iron boron magnetic body, then is cleaned by ultrasonic 3 times with absolute ethyl alcohol, by the neodymium iron boron magnetic body after ultrasonic cleaning
10min is soaked in absolute ethyl alcohol, is finally dried up.
(3) preparation of alcohol radical inorganic composite coating：Magnet surface first after the pre-treatment spray one layer of subbing (by
The alcohol radical inorganic compounding coating that with the addition of the anticracking powder of mass percent 3% is formed), 5 minutes levellings are stored at room temperature after spraying, then
An aspect coating (the alcohol radical inorganic compounding coating as prepared) is sprayed again, is stored at room temperature 5 minutes levellings, then carry out at drying
Reason, including 15min is toasted at a temperature of 120 DEG C, and toast 30min at a temperature of 250 DEG C.
Embodiment 4
(1) preparation of alcohol radical inorganic compounding coating：According to 5:1 mass ratio by mass fraction be 6% Ludox and matter
Measure the nano-TiO that fraction is 4%2Colloidal sol is well mixed under 300r/min stir speed (S.S.)s, is then added and Ludox mass ratio
For 1:4 titanate esters (mass ratio 1:1 purity titanium tetraethoxide and butyl titanate), use mass fraction for 6% hydrochloric acid water
Solution regulation system pH value is 3, reacts 2h at room temperature；In the case where continuing stirring condition, it is 6 to add with titanate esters mass ratio:1
Tetraethoxysilane, and add with tetraethoxysilane mass ratio be 8:1 alcoholic solvent (volume ratio 3:1 ethanol and two
Pyruvic alcohol), while the ammoniacal liquor that mass fraction is 25% is added, it is 4 to make the mol ratio of ammoniacal liquor and element silicon:1, stirred at 60 DEG C
9h is reacted, forms silicon titanium complex sol；Afterwards, according to 10:1:4 mass ratio is by above-mentioned silicon titanium complex sol, inorganic filler (matter
Amount is than being 1:1:1:2 Al powder, titanium dioxide, alumina powder and graphite powder, granularity are 2000 mesh) and alcoholic solvent (volume ratio 2:1
Ethanol and isopropanol) be added to sand mill, be ground 5h, prepare alcohol radical inorganic compounding coating.
(2) neodymium iron boron magnetic body surface preparation：Prepare neodymium iron boron magnetic body sample (50mm × 50mm × 5mm) first, it is first right
Neodymium iron boron magnetic body carries out chamfered, polishing derusting is carried out respectively with 150# sand paper and 600# sand paper, afterwards with 1.5% dust technology
Pickling processes 10s is carried out to neodymium iron boron magnetic body, then is cleaned by ultrasonic 3 times with absolute ethyl alcohol, by the neodymium iron boron magnetic body after ultrasonic cleaning
10min is soaked in absolute ethyl alcohol, is finally dried up.
(3) preparation of alcohol radical inorganic composite coating：Magnet surface first after the pre-treatment spray one layer of subbing (by
The alcohol radical inorganic compounding coating that with the addition of the anticracking powder of mass percent 4% is formed), 8 minutes levellings are stored at room temperature after spraying, then
An aspect coating (the alcohol radical inorganic compounding coating as prepared) is sprayed again, is stored at room temperature 8 minutes levellings, then carry out at drying
Reason, including 10min is toasted at a temperature of 170 DEG C, and toast 90min at a temperature of 150 DEG C.
Comparative example 1
It is same as Example 1, in addition to not adding inorganic filler.
It is as follows using the resistance to middle salt acid mist performance of the testing coating of resistance to neutral salt spray test commonly used in the art, test result
Table 1：
Table 1
| Embodiment | Coating layer thickness | Testing time | Corrosion situation |
| 1 | 15μm | 1200h | Not corrosion |
| 2 | 17μm | 1300h | Not corrosion |
| 3 | 20μm | 1200h | Not corrosion |
| 4 | 18μm | 1300h | Not corrosion |
| Comparative example 1 | 15μm | 1200h | Corrosion |
From the test result of the embodiment 1 in upper table 1 to embodiment 4, the alcohol radical prepared using the method for the present invention
Inorganic composite coating can effectively improve the corrosion resistance of coating, and in more than 1000h corrosion does not occur for the resistance to neutral salt spray time；This is
Because the addition of the crystalline inorganic filler of addition causes the corrosion resistance of the alcohol radical inorganic composite coating to be improved, and including aluminium
One or more granularities in powder, silver powder, alumina powder, oxide powder and zinc, titanium dioxide, graphite powder and silica flour for 100~
The crystalline inorganic filler of 2000 mesh can be dispersed in amorphous inorganic colloidal sol, effectively combined with amorphous inorganic colloidal sol,
So as to effectively improve the corrosion resistance of coating.
From embodiment 1 and the test result of comparative example 1, when not adding crystalline inorganic filler in coating, the then painting
Corrosion easily occurs for layer, further demonstrates that the addition of crystalline inorganic filler improves the corrosion resistance of coating.
In addition, by the present invention in that the basic knot of coating is formed with the amorphous inorganic colloidal sol in three-dimensional netted cross structure
Structure, the structure allow amorphous inorganic colloidal sol to be combined closely with neodymium-iron-boron body interface, further increase the coating with
The adhesion of neodymium iron boron magnetic body, and the institutional framework of the alcohol radical inorganic composite coating is crystalline state and amorphous-state composite structures or crystalline substance
State composite construction, it can effectively prevent the coating surface from aoxidizing.
To sum up, by alcohol radical inorganic composite coating prepared by method of the invention without chromium, without toxic solvent, without a huge sum of money
Category pollution, it can effectively solve the problem that neodymium iron boron magnetic body is electroplated, chemical plating process of surface treatment is brought problem of environmental pollution and application
On limitation, can apply to Nd-Fe-B magnetic material surfacecti proteon field.
It will be understood by those skilled in the art that above example is only exemplary embodiment, in the spirit without departing substantially from the present invention
In the case of scope, a variety of changes can be carried out, replaces and changes.
Claims (11)
1. a kind of alcohol radical inorganic composite coating, it is characterised in that the alcohol radical inorganic composite coating is by inorganic sol and inorganic fills out
Material composition, wherein, the inorganic sol includes Ludox, TiO 2 sol and alkoxy silane and metatitanic acid ester hydrolysis produces
Thing, the inorganic filler include one kind in aluminium powder, silver powder, alumina powder, oxide powder and zinc, titanium dioxide, graphite powder and silica flour
It is or a variety of.
2. a kind of alcohol radical inorganic composite coating according to claim 1, wherein, the tissue of the alcohol radical inorganic composite coating
Structure is crystalline state and amorphous-state composite structures or crystalline state composite construction.
A kind of 3. method for preparing alcohol radical inorganic composite coating, it is characterised in that comprise the following steps：
Ludox and TiO 2 sol are mixed；
Titanate esters and aqueous hydrochloric acid solution are added, pH is adjusted, reaction, adds alkoxy silane and the first alcoholic solvent and ammoniacal liquor,
Reaction, obtains silicon titanium complex sol；
The silicon titanium complex sol and inorganic filler are added in the second alcoholic solvent, obtain alcohol radical inorganic compounding coating；And
The alcohol radical inorganic compounding coating is sprayed, alcohol radical inorganic composite coating is prepared.
4. according to the method for claim 3, wherein, the Ludox is the silica for 40~80nm by average grain diameter
The dispersion formed in one or more dispersion solvents in ethanol, isopropanol, n-butanol and DAA；The dioxy
Change titanium colloidal sol be by average grain diameter be 20~50nm nano titanium oxide in ethanol, isopropanol, n-butanol and DAA
One or more dispersion solvents in the dispersion that is formed.
5. according to the method for claim 3, wherein, the mass fraction of the silica in the Ludox for 5%~
10%, the mass fraction of the titanium dioxide in the TiO 2 sol is 3%~5%.
6. according to the method for claim 3, wherein, the titanate esters include purity titanium tetraethoxide, butyl titanate and metatitanic acid
One or more in four isopropyl esters；First alcoholic solvent and second alcoholic solvent include alcohol solvent, isopropanol respectively
One or more in solvent, n-butanol solvent and DAA solvent.
7. according to the method for claim 3, wherein, the inorganic filler includes aluminium powder, silver powder, alumina powder, zinc oxide
One or more in powder, titanium dioxide, graphite powder and silica flour, the granularity of the inorganic filler is 100~2000 mesh.
8. the method according to claim 11, in addition to：Before the alcohol radical inorganic compounding coating is sprayed, first
Chamfered is carried out to magnet, then carries out polishing derusting with emery cloth, carries out pickling processes to magnet with nitric acid afterwards, then with nothing
Water-ethanol is cleaned by ultrasonic, and the magnet after ultrasonic cleaning is soaked in absolute ethyl alcohol.
9. according to the method for claim 3, wherein, it is described the alcohol radical inorganic compounding coating is subjected to spraying to include：Adopt
Sprayed with the magnet surface of layering spraying method after the pre-treatment, magnet surface first after the pre-treatment sprays one layer of bottom
Coating；Then an aspect coating is sprayed on the subbing subbing, then carries out drying and processing.
10. according to the method for claim 9, wherein, the subbing is applied by anticracking powder and the alcohol radical inorganic compounding
Material is formed, and the investment precoat is the alcohol radical inorganic compounding coating,
Wherein, the mass percent that the anticracking powder accounts for the gross mass of the subbing is 3%~5%.
11. according to the method for claim 9, wherein, the drying and processing includes being pre-reacted to mem stage and low temperature successively
In the sintering reaction stage, the mem stage that is pre-reacted to is anti-using 80 DEG C~170 DEG C 10~30min of baking, the low-temperature sintering
It should be using 150 DEG C~250 DEG C 30~90min of baking in the stage.
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| CN108659581A (en) * | 2018-04-27 | 2018-10-16 | 成都今天化工有限公司 | A method of preparing super abrasive nano-titanium porcelain coating |
| CN110804396A (en) * | 2019-12-09 | 2020-02-18 | 万华化学集团股份有限公司 | Anticorrosive paint and preparation method and application thereof |
| CN111592780A (en) * | 2020-06-08 | 2020-08-28 | 青岛浩普凯诚环保新材料有限公司 | High-speed train shell protection liquid and preparation method thereof |
| CN112138967A (en) * | 2020-09-15 | 2020-12-29 | 宁波太尔炊具有限公司 | Preparation method of wear-resistant ceramic coating non-stick pan |
| CN115537796A (en) * | 2022-09-02 | 2022-12-30 | 中国科学院宁波材料技术与工程研究所 | Surface protection method of sintered neodymium-iron-boron magnet and product thereof |
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| CN108659581A (en) * | 2018-04-27 | 2018-10-16 | 成都今天化工有限公司 | A method of preparing super abrasive nano-titanium porcelain coating |
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| CN112138967A (en) * | 2020-09-15 | 2020-12-29 | 宁波太尔炊具有限公司 | Preparation method of wear-resistant ceramic coating non-stick pan |
| CN112138967B (en) * | 2020-09-15 | 2022-05-17 | 宁波太尔炊具有限公司 | Preparation method of wear-resistant ceramic coating non-stick pan |
| CN115537796A (en) * | 2022-09-02 | 2022-12-30 | 中国科学院宁波材料技术与工程研究所 | Surface protection method of sintered neodymium-iron-boron magnet and product thereof |
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