CN102443834A - Preparation method of particle-enhanced organic anticorrosive coating on surface of neodymium-iron-boron permanent magnet material - Google Patents
Preparation method of particle-enhanced organic anticorrosive coating on surface of neodymium-iron-boron permanent magnet material Download PDFInfo
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Abstract
The invention relates to a preparation method of a particle-enhanced organic anticorrosive coating on the surface of a neodymium-iron-boron permanent magnet material, and specifically relates to a cathode electrophoresis coating method of the particle-enhanced organic anticorrosive coating on the surface of the neodymium-iron-boron permanent magnet material. According to the invention, first, the surface of the neodymium-iron-boron permanent magnet material is polished; the surface of the neodymium-iron-boron permanent magnet material is subject to degreasing, rust removing by acid cleaning, surface phosphorizing, cathode electrophoresis coating and high-temperature curing, such that a particle-enhanced organic matter coating is formed on the surface of the neodymium-iron-boron permanent magnet material. According to the coating provided by the invention, epoxy resin, acrylic acid and polyurethane are adopted as substrates; micro-nano titanium oxide particles, alumina particles, graphite particles, aluminum particles and the like are adopted as enhancing phases, such that a composite organic coating can be prepared. The coating causes no influence on the inherent magnetic performance of the magnet. The coating has a good bonding force with the magnet, and has a good caking property with bonding glue. The coating is also advantaged in uniform thickness, smooth surface, high corrosion resistance, and low preparation cost.
Description
Technical field
The present invention relates to the surface electrochemistry process field of material, especially the neodymium-iron-boron permanent magnetic material surface particle strengthens the cathode electro-coating method of organic anti-corrosive coating.
Background technology
The NdFeB permanent magnet has obtained using widely in fields such as microwave technology, audio-visual technology, electrical engineering, instrumental technique, computer technology, magnetic separation technique, biotechnology, automotive industrys owing to its outstanding magnetic property since nineteen eighty-three is born, and the NdFeB industry has become the important component part of the national economic development.But its corrosion resistance is relatively poor, has limited its range of application widely.Therefore, how to improve the major issue that its corrosion resistance becomes NdFeB material production and use.The treatment process that improves at present NdFeB permanent magnet material corrosion resistance nature is summed up and is mainly contained two types: the one, magnetic is directly handled, i.e. alloying; The 2nd, finished product is applied, i.e. surfacecti proteon is handled.The effect of alloying is more limited, and adds alloying element and can to a certain degree reduce the magnet magnetic property, can form like Co and stablize that crystal boundary improves solidity to corrosion mutually but the adding to join and reduced the coercive force and the magnetic energy product of magnet itself of Co.So surfacecti proteon is treated as and improves the most effectively way of NdFeB permanent magnet material corrosion resistance nature.At present; Mainly contain sufacings such as bonderizing, plating, electrophoretic coating, electroless plating, magnetron sputtering, ion plating, rare-earth conversion coatings, sol-gel applies in the protection of NdFeB permanent magnet material independent or compoundly; The wherein successful commercialization of electrophoresis application technique has improved the solidity to corrosion of neodymium iron boron effectively.The present invention carries out the particle enhancing through in electrophoresis liquid such as epoxy resin, vinylformic acid, urethane, adding particles such as micro/nano level titanium oxide, aluminum oxide, graphite, aluminium to the electrophoresis organic coating; Can further improve the solidity to corrosion and the use temperature that improves coating of magnet, prolong the work-ing life of NdFeB material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of surface of Nd-Fe-B permanent magnet particle enhancing organic anti-corrosive coating, for solidity to corrosion difference and the further solidity to corrosion of electrophoresis organic coating and the problem of use temperature of improving that solves neodymium iron boron.
The present invention realizes that so said preparation method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out surface grinding and handle;
(2) degreasing degreasing: the grinded magnet of chamfering is put into alkaline degreaser carry out degreasing degreasing;
(3) acid pickling and rust removing: put into acidic solution and carry out acid pickling and rust removing;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into phosphatization liquid carry out the alramenting processing, phosphatization adopts middle temperature phosphating, and temperature is 50 ~ 75 ℃, and the treatment time is 5 ~ 15min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out cathode electro-coating;
(6) hot setting: the magnet after the application carries out hot setting after room temperature leaves standstill 15min in clean environment, finally forms particle at surface of Nd-Fe-B permanent magnet and strengthens organic coating.
Said neodymium iron boron can be sintered NdFeB or Agglutinate neodymium-iron-boron.
Said acidic solution can be hydrochloric acid or sulfuric acid or nitric acid or other mixing acid, concentration massfraction 10 ~ 40%HCl pickling 5～60s, massfraction 10 ~ 40%HNO
3Pickling 10～60s, massfraction 10～40%H
2SO
4Pickling 5 ~ 60s.
Said phosphatization liquid can be any one in zinc system, zinc calcium system, zinc-manganese system, manganese system, iron system and the amorphous phase iron.
Said electrophoresis liquid is epoxy resin or vinylformic acid or urethane electrophoresis with organism with through the aqueous solution of tensio-active agent activatory granulometric composition, and the mass ratio of its organism and water is 1:2 ~ 1:8, and granule density is 30 ~ 200g/L.
Said particle is titanium oxide, aluminium sesquioxide, graphite or aluminium, and particle grain size is 50 ~ 200nm.
Also have organism such as some flow agents, skimmer and tensio-active agent in the said electrophoresis liquid, the amount mark that accounts for total raw material is 0.1～1% esters of acrylic acid flow agent, 0.1%-0.3% ZX-I dipersant, 0.5 ~ 0.8% phosphoric acid ester skimmer.
The electrophoretic voltage of said cathode electro-coating is 20 ~ 60 V, and electrophoresis time is 10 ~ 60 s, and the electrophoresis liquid temperature is controlled at 20 ~ 35 ℃.
The solidification value of said hot setting is 160～180 ℃, and be 30～60min set time.
The present invention can obtain particle at surface of Nd-Fe-B permanent magnet and strengthen the organic anti-corrosive coating, and it evenly is 10～30 μ m that coating does not have influence, thickness to Nd-Fe-B permanent magnet inherent magnetic property, defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle; The cross-hatching sticking power of coating and Nd-Fe-Bo permanent magnet material can reach 0 grade; The coating cohesive force can reach more than the 15MPa, and pencil hardness is 2H～4H, salt-fog resistant test>600h; Anti-PCT test>600h, humid heat test>700h.
Preparing method of the present invention realizes that industrial application is simple, and production cost is low, and the product price ratio is high; Application does not receive the influence of magnet material contour structures; Environmentally safe can improve the solidity to corrosion of neodymium iron boron magnetic body and the use temperature of raising organic coating effectively, prolongs the work-ing life of magnet.
Description of drawings
The surperficial SEM photo that Fig. 1 is obtained for embodiment 2.
Embodiment
Embodiment 1
The preparation method that this embodiment surface of Nd-Fe-B permanent magnet particle strengthens the organic anti-corrosive coating carries out according to the following steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that the 38SH sintered Nd-Fe-B permanent magnet is carried out surface grinding and handle, final size is 25 * 12 * 3mm;
(2) degreasing degreasing: the grinded magnet of chamfering is put into 60 ℃ of alkaline degreasers (staple is yellow soda ash, sodium phosphate, water glass and emulsifying agent etc.) carry out the 5min degreasing degreasing;
(3) acid pickling and rust removing: put into 10% HNO
3Solution carries out acid pickling and rust removing 10s;
(4) alramenting: put into Zinc phosphating solution to the permanent magnet behind the acid pickling and rust removing and carry out 60～70 ℃ of middle temperature phosphatings and handle 2 min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out cathode electro-coating; Wherein the mass ratio of the epoxy resin of electrophoresis liquid and zero(ppm) water is 1:3; Titanium dioxide granule concentration is 50g/L, and particle diameter is 100 ~ 200nm, and electrophoretic voltage is 50V; Electrophoresis time is 50s, is 30 ± 2 ℃ through heating in water bath control electrophoresis liquid temperature;
(6) hot setting: the magnet after the application carries out 160 ℃ of hot setting 50min after room temperature leaves standstill 15min in clean environment, finally forms white titanium dioxide granule reinforced epoxy coating at surface of Nd-Fe-B permanent magnet.
The coat-thickness that this embodiment obtains is ~ 20 μ m; Defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle, the cross-hatching sticking power of coating and magnet material can reach 0 grade, and the cohesive force of coating can reach 20MPa; Pencil hardness is 3H; Salt-fog resistant test>1000h, anti-PCT test>1000h, humid heat test>1000h.
Embodiment 2
The preparation method that this embodiment surface of Nd-Fe-B permanent magnet particle strengthens the organic anti-corrosive coating carries out according to the following steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that the 30EH sintered Nd-Fe-B permanent magnet is carried out surface grinding and handle, final size is 40 * 50 * 10mm;
(2) degreasing degreasing: the grinded magnet of chamfering is put into 60 ℃ of alkaline degreasers (mainly become and be yellow soda ash, sodium phosphate, water glass and emulsifying agent etc.) carry out the 5min degreasing degreasing;
(3) acid pickling and rust removing: put into the 0.25mol/L sulphuric acid soln and carry out acid pickling and rust removing 10s;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into Zinc phosphating solution carry out the surface and adopt 60～70 ℃ of middle temperature phosphatings to handle 2 min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out the surface and carry out cathode electro-coating; Wherein the mass ratio of the vinylformic acid of electrophoresis liquid and zero(ppm) water is 1:8; Titanium dioxide granule concentration is 120g/L, and particle diameter is 100 ~ 200nm, and electrophoretic voltage is 60V; Electrophoresis time is 50s, is 30 ± 2 ℃ through heating in water bath control electrophoresis liquid temperature;
(6) hot setting: the magnet after the application carries out 170 ℃ of hot setting 50min after room temperature leaves standstill 15min in clean environment, finally forms white titanium dioxide granule at surface of Nd-Fe-B permanent magnet and strengthens acrylic acid coatings.
The coat-thickness that this embodiment obtains is ~ 25 μ m, defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle, and the cross-hatching sticking power of coating and magnet material can reach 0 grade; The cohesive force of coating can reach 16MPa; Pencil hardness is 4H, salt-fog resistant test>800h, anti-PCT test>800h; Humid heat test>900h, see shown in Figure 2.
Embodiment 3
The preparation method that this embodiment surface of Nd-Fe-B permanent magnet particle strengthens the organic anti-corrosive coating carries out according to the following steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that the 30EH sintered Nd-Fe-B permanent magnet is carried out surface grinding and handle, final size is 40 * 50 * 10mm;
(2) degreasing degreasing: the grinded magnet of chamfering is put into 60 ℃ of alkaline degreasers (mainly become and be yellow soda ash, sodium phosphate, water glass and emulsifying agent etc.) carry out the 5min degreasing degreasing;
(3) acid pickling and rust removing: put into the 0.25mol/L sulphuric acid soln and carry out acid pickling and rust removing 10s;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into Zinc phosphating solution carry out the surface and adopt 60～70 ℃ of middle temperature phosphatings to handle 2 min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out the surface and carry out cathode electro-coating; Wherein the mass ratio of the vinylformic acid of electrophoresis liquid and zero(ppm) water is 1:8; Alumina particle concentration is 150g/L, and particle diameter is 100 ~ 150nm, and electrophoretic voltage is 70V; Electrophoresis time is 50s, is 30 ± 2 ℃ through heating in water bath control electrophoresis liquid temperature;
(6) hot setting: the magnet after the application carries out 170 ℃ of hot setting 50min after room temperature leaves standstill 15min in clean environment, finally forms the white alumina particle at surface of Nd-Fe-B permanent magnet and strengthens acrylic acid coatings.
The coat-thickness that this embodiment obtains is ~ 25 μ m; Defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle, the cross-hatching sticking power of coating and magnet material can reach 0 grade, and the cohesive force of coating can reach 16MPa; Pencil hardness is 4H; Salt-fog resistant test>800h, anti-PCT test>900h, humid heat test>1000h.
Embodiment 4
The preparation method that this embodiment surface of Nd-Fe-B permanent magnet particle strengthens the organic anti-corrosive coating carries out according to the following steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that the 28AH sintered Nd-Fe-B permanent magnet is carried out surface grinding and handle, final size is Φ 30 * 50mm;
(2) degreasing degreasing: the grinded magnet of chamfering is put into 60 ℃ of alkaline degreasers (mainly become and be yellow soda ash, sodium phosphate, water glass and emulsifying agent etc.) carry out the 5min degreasing degreasing;
(3) acid pickling and rust removing: put into 15% HNO
3Solution carries out acid pickling and rust removing 10s;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into Zinc phosphating solution carry out the surface and adopt 60～70 ℃ of middle temperature phosphatings to handle 2 min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out the surface and carry out cathode electro-coating; Wherein the mass ratio of the urethane of electrophoresis liquid and zero(ppm) water is 1:7; Titanium dioxide granule concentration is 150g/L, and particle diameter is 100 ~ 200nm, and electrophoretic voltage is 50V; Electrophoresis time is 60s, is 30 ± 2 ℃ through heating in water bath control electrophoresis liquid temperature;
(6) hot setting: the magnet after the application carries out 170 ℃ of hot setting 60min after room temperature leaves standstill 15min in clean environment, finally forms white titanium dioxide granule at surface of Nd-Fe-B permanent magnet and strengthens polyurethane coating.
The coat-thickness that this embodiment obtains is ~ 20 μ m; Defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle, the cross-hatching sticking power of coating and magnet material can reach 0 grade, and the cohesive force of coating can reach 16MPa; Pencil hardness is 3H; Salt-fog resistant test>700h, anti-PCT test>700h, humid heat test>700h.
Embodiment 5
The preparation method that this embodiment surface of Nd-Fe-B permanent magnet particle strengthens the organic anti-corrosive coating carries out according to the following steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that the 28AH sintered Nd-Fe-B permanent magnet is carried out surface grinding and handle, final size is Φ 30 * 50mm;
(2) degreasing degreasing: the grinded magnet of chamfering is put into 60 ℃ of alkaline degreasers (mainly become and be yellow soda ash, sodium phosphate, water glass and emulsifying agent etc.) carry out the 5min degreasing degreasing;
(3) acid pickling and rust removing: put into 15% HNO
3Solution carries out acid pickling and rust removing 10s;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into Zinc phosphating solution carry out the surface and adopt 60～70 ℃ of middle temperature phosphatings to handle 2 min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out the surface and carry out cathode electro-coating; Wherein the mass ratio of the epoxy resin of electrophoresis liquid and zero(ppm) water is 1:2.5; Graphite granule concentration is 180g/L, and particle diameter is 100 ~ 150nm, and electrophoretic voltage is 40V; Electrophoresis time is 30s, is 30 ± 2 ℃ through heating in water bath control electrophoresis liquid temperature;
(6) hot setting: the magnet after the application carries out 180 ℃ of hot setting 40min after room temperature leaves standstill 15min in clean environment, finally forms the graphite granule reinforced epoxy coating of black at surface of Nd-Fe-B permanent magnet.
The coat-thickness that this embodiment obtains is ~ 20 μ m; Defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle, the cross-hatching sticking power of coating and magnet material can reach 0 grade, and the cohesive force of coating can reach 17MPa; Pencil hardness is 2H; Salt-fog resistant test>1000h, anti-PCT test>1000h, humid heat test>1000h.
Embodiment 6
The preparation method that this embodiment surface of Nd-Fe-B permanent magnet particle strengthens the organic anti-corrosive coating carries out according to the following steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that the 28AH sintered Nd-Fe-B permanent magnet is carried out surface grinding and handle, final size is Φ 30 * 50mm;
(2) degreasing degreasing: the grinded magnet of chamfering is put into 60 ℃ of alkaline degreasers (mainly become and be yellow soda ash, sodium phosphate, water glass and emulsifying agent etc.) carry out the 5min degreasing degreasing;
(3) acid pickling and rust removing: put into 15% HNO
3Solution carries out acid pickling and rust removing 10s;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into Zinc phosphating solution carry out the surface and adopt 60～70 ℃ of middle temperature phosphatings to handle 2 min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out the surface and carry out cathode electro-coating; Wherein the mass ratio of the epoxy resin of electrophoresis liquid and zero(ppm) water is 1:3; Al particulate concentration is 100g/L, and particle diameter is 500 ~ 100nm, and electrophoretic voltage is 50V; Electrophoresis time is 30s, is 30 ± 2 ℃ through heating in water bath control electrophoresis liquid temperature;
(6) hot setting: the magnet after the application carries out 170 ℃ of hot setting 40min after room temperature leaves standstill 15min in clean environment, finally forms silver-gray al particulate reinforced epoxy coating at surface of Nd-Fe-B permanent magnet.
The coat-thickness that this embodiment obtains is ~ 25 μ m; Defectives such as the no shrinkage cavity in surface, pore, pin hole, orange peel and particle, the cross-hatching sticking power of coating and magnet material can reach 0 grade, and the cohesive force of coating can reach 18MPa; Pencil hardness is 3H; Salt-fog resistant test>1000h, anti-PCT test>1000h, humid heat test>1000h.
Though introduce and described embodiment of the present invention, the present invention is not limited thereto, but can also come concrete realization with other modes in the scope that is in the technical scheme that defines in the accompanying claims.
Claims (9)
1. the preparation method of a neodymium-iron-boron permanent magnetic material surface particle enhancing organic anti-corrosive coating is characterized in that said preparation method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out surface grinding and handle;
(2) degreasing degreasing: the grinded magnet of chamfering is put into alkaline degreaser carry out degreasing degreasing;
(3) acid pickling and rust removing: put into acidic solution and carry out acid pickling and rust removing;
(4) alramenting: the permanent magnet behind the acid pickling and rust removing is put into phosphatization liquid carry out the alramenting processing, phosphatization adopts middle temperature phosphating, and temperature is 50 ~ 75 ℃, and the treatment time is 5 ~ 15min;
(5) ability cathode electrophoresis: the permanent magnet behind the bonderizing is put into electrophoresis liquid carry out cathode electro-coating;
(6) hot setting: the magnet after the application carries out hot setting after room temperature leaves standstill 15min in clean environment, finally forms particle at surface of Nd-Fe-B permanent magnet and strengthens organic coating.
2. surface of Nd-Fe-B permanent magnet particle according to claim 1 strengthens the preparation method of organic anti-corrosive coating, it is characterized in that said neodymium iron boron can be sintered NdFeB or Agglutinate neodymium-iron-boron.
3. surface of Nd-Fe-B permanent magnet particle according to claim 1 strengthens the preparation method of organic anti-corrosive coating; It is characterized in that said acidic solution can be hydrochloric acid or sulfuric acid or nitric acid or other mixing acid; Concentration massfraction 10 ~ 40%HCl pickling 5～60s, massfraction 10 ~ 40%HNO
3Pickling 10～60s, massfraction 10～40%H
2SO
4Pickling 5 ~ 60s.
4. surface of Nd-Fe-B permanent magnet particle according to claim 1 strengthens the preparation method of organic anti-corrosive coating, it is characterized in that said phosphatization liquid can be any one in zinc system, zinc calcium system, zinc-manganese system, manganese system, iron system and the amorphous phase iron.
5. surface of Nd-Fe-B permanent magnet particle according to claim 1 strengthens the preparation method of organic anti-corrosive coating; It is characterized in that said electrophoresis liquid is epoxy resin or vinylformic acid or urethane electrophoresis with organism with through the aqueous solution of tensio-active agent activatory granulometric composition; The mass ratio of its organism and water is 1:2 ~ 1:8, and granule density is 30 ~ 200g/L.
6. surface of Nd-Fe-B permanent magnet particle according to claim 5 strengthens the preparation method of organic anti-corrosive coating, it is characterized in that said particle is titanium oxide, aluminium sesquioxide, graphite or aluminium, and particle grain size is 50 ~ 200nm.
7. surface of Nd-Fe-B permanent magnet particle according to claim 1 strengthens the preparation method of organic anti-corrosive coating; It is characterized in that also existing in the said electrophoresis liquid organism such as some flow agents, skimmer and tensio-active agent; The amount mark that accounts for total raw material is 0.1～1% esters of acrylic acid flow agent; 0.1%-0.3% ZX-I dipersant, 0.5 ~ 0.8% phosphoric acid ester skimmer.
8. surface of Nd-Fe-B permanent magnet particle according to claim 1 strengthens the preparation method of organic anti-corrosive coating, and the electrophoretic voltage that it is characterized in that said cathode electro-coating is 20 ~ 60 V, and electrophoresis time is 10 ~ 60 s, and the electrophoresis liquid temperature is controlled at 20 ~ 35 ℃.
9. strengthen the preparation method of organic anti-corrosive coating according to the surface of Nd-Fe-B permanent magnet particle of claim 1, the solidification value that it is characterized in that said hot setting is 160～180 ℃, and be 30～60min set time.
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