CN102397835A - Method for performing surface treatment on neodymium-iron-boron permanent magnet material by using nano ceramic - Google Patents
Method for performing surface treatment on neodymium-iron-boron permanent magnet material by using nano ceramic Download PDFInfo
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Abstract
The invention provides a method for performing surface treatment on a neodymium-iron-boron permanent magnet material by using nano ceramic. The method comprises the following steps of: (1) polishing chamfers; (2) degreasing and removing oil; (3) acid-washing and derusting; (4) treating by using the nano ceramic, namely putting the neodymium-iron-boron permanent magnet material into a nano ceramic plating solution and performing nano ceramic treatment, wherein the nano ceramic plating solution comprises a main film-forming agent, a film-forming aid, a filler and a curing agent, the main film-forming agent is epoxy resin with an amino group or an epoxy group, the film-forming aid is at least one of methyl isobutyl ketone, methyl ethyl ketone peroxide and tert-butyl peroxyacetate, the filler is nano-silicon dioxide and/or alumina, and the curing agent is triethanolamine and/or diethanolamine; and (5) washing and blow-drying to solidify a nano ceramic plated layer. By the surface treatment method, the neodymium-iron-boron permanent magnet material can obtain excellent corrosion resistance, and the high-temperature demagnetization rate of the neodymium-iron-boron permanent magnet material is greatly reduced.
Description
Technical field
The present invention relates to a kind of surface treatment method of Nd-Fe-Bo permanent magnet material, relate to a kind of employing nano ceramics especially Nd-Fe-Bo permanent magnet material is carried out the surface-treated method.
Background technology
Application of neodymium iron boron (NdFeB) permanent-magnet material in recent years and development very rapidly, and the protection of Nd-Fe-Bo permanent magnet material is to be related to one of key technology that can Nd-Fe-Bo permanent magnet material apply.Nd-Fe-Bo permanent magnet material mainly is prepared from through powder metallurgical technique elements such as rare earth metal neodymium (Nd), iron and boron.As the strongest present magnetic material, Nd-Fe-Bo permanent magnet material has been widely used in fields such as electroplating device, machinery, medical treatment, automobile, and application prospect is very wide.
The prerequisite that Nd-Fe-Bo permanent magnet material is used is at first to resolve the anticorrosion problem of Nd-Fe-Bo permanent magnet material.As a kind of porous material that is prepared from powder metallurgical technique, rich neodymium phase, neodymium iron boron principal phase and borderline phase in the Nd-Fe-Bo permanent magnet material are easy to form intercrystalline corrosion.Because the character of the rear earth element nd in the neodymium iron boron powder alloy is active; Thereby the corrosion resisting property that makes whole Nd Fe B alloys becomes very poor; Particularly very easily corrosion in damp and hot environment; And, had a strong impact on the service life of Nd-Fe-Bo permanent magnet material because of corrosion failure causes the decline or the damage of magnetic property, reduced the stability and the reliability of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its institutional framework have very big relation.The principal phase of Nd-Fe-Bo permanent magnet material is the main source of its magnetic property, and to coercivity contribution maximum be rich neodymium phase.After Nd-Fe-Bo permanent magnet material corrodes, huge variation will take place in its magnetic property.Therefore, the anticorrosion problem of Nd-Fe-Bo permanent magnet material is the subject matter that Nd-Fe-Bo permanent magnet material need solve always.
At present, the anti-corrosion method of Nd-Fe-Bo permanent magnet material has a variety of, for example electronickelling, electrogalvanizing (CN1421547A, CN1056133A), plating MULTI-LAYER NICKEL, copper facing (CN1514889A), phosphatization, electrophoretic paint etc.Electrogalvanizing is under the effect of dc source, and the metallic zinc ion is reduced into metallic zinc on negative electrode.
On the other hand, how to reduce the flux loss of Nd-Fe-Bo permanent magnet material in surface treatment process and more and more become a sharp-pointed problem.Measure the magnetic flux of the Nd-Fe-Bo permanent magnet material of film forming, after under 150 ℃ this Nd-Fe-Bo permanent magnet material placement being cooled to normal temperature after 1 hour, so repeating 2-3 time, measure the flux value of this Nd-Fe-Bo permanent magnet material more then.Flux value according to this twice measurement can calculate the high temperature demagnetize.High temperature demagnetize through the Nd-Fe-Bo permanent magnet material after the surface treatment method processing of the prior art is generally 2-15%.
Summary of the invention
The object of the present invention is to provide a kind of employing nano ceramics that Nd-Fe-Bo permanent magnet material is carried out surface treatment method, said method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: use sodium phosphate, sodium carbonate or NaOH that said Nd-Fe-Bo permanent magnet material is carried out conventional degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that said Nd-Fe-Bo permanent magnet material is carried out conventional acid pickling and rust removing, washing then;
(4) nano ceramics is handled: said Nd-Fe-Bo permanent magnet material is put into the nano ceramics plating bath carry out the nano ceramics processing, said nano ceramics plating bath comprises main film forming agent, coalescents, filler and curing agent; Wherein, Said main film forming agent is the epoxy resin that has amino or epoxy radicals; Said coalescents is selected from least a in methyl iso-butyl ketone (MIBK), methyl ethyl ketone peroxide and the peroxidating acetate uncle fourth fat; Said filler is nano silicon and/or aluminium oxide, and said curing agent is triethanolamine and/or diethanol amine; With
(5) wash, dry up, with the curing nano ceramic plated layer.
Preferably, said main film forming agent is E-44 epoxy resin or E-51 epoxy resin.
Preferably, the content of said main film forming agent is the 15-25 gram.
Preferably, the content of said coalescents is the 5-25 gram.
Preferably, the content of said filler is the 50-65 gram.
Preferably, the content of said curing agent is the 5-20 gram.
Preferably, said nano ceramics is handled and is carried out at normal temperatures.
Preferably, solidification temperature is 120 ℃, and be 1.5 hours hardening time.
Preferably, said Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
In surface treatment method of the present invention, at first Nd-Fe-Bo permanent magnet material is carried out surface treatment, this surface treatment can adopt known method of the prior art to carry out.For example, at first use mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is polished.Use alkaline solution that Nd-Fe-Bo permanent magnet material is carried out degreasing degreasing then, for example Nd-Fe-Bo permanent magnet material is put into the alkaline solution that NaOH that the sodium phosphate that risen by 20g/, sodium carbonate that 10g/ rises and 10g/ rise forms and carry out degreasing degreasing.Then this Nd-Fe-Bo permanent magnet material is carried out acid pickling and rust removing, for example use the salpeter solution of 1% (volume ratio) to clean the oxide of removing this neodymium-iron-boron permanent magnetic material surface.Final rinse water falls the acid and the impurity of neodymium-iron-boron permanent magnetic material surface.
Surface treatment method provided by the present invention is to be that primary raw material carries out surface treatment to Nd-Fe-Bo permanent magnet material with epoxy resin and some inorganic fillers, and this surface treatment method does not use phosphorus, and in processing procedure, does not produce sediment, therefore has the advantage of environmental protection.Simultaneously, method of the present invention can be carried out at normal temperatures, need not to heat, and the processing time is short, control is easy, can save table and transfer operation, and tank liquor is reusable.Compare with the phosphatization surface treatment, surface treatment method of the present invention can reduce by 15～30% with cost.
The surface treatment method of the application of the invention can make Nd-Fe-Bo permanent magnet material obtain the superior corrosion resistance ability.Simultaneously, another beneficial effect of surface treatment method of the present invention is the high temperature demagnetizing factor that greatly reduces Nd-Fe-Bo permanent magnet material, and the high temperature demagnetizing factor is controlled at below 0.01%.
The specific embodiment
In order further to understand structure of the present invention, characteristic and other purposes, combine appended preferred embodiment to specify as follows at present, illustrated preferred embodiment only is used to technical scheme of the present invention is described, and non-limiting the present invention.
Embodiment 1
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, nano ceramics is handled.Wherein main film forming agent is E-51 epoxy resin 15 grams, methyl iso-butyl ketone (MIBK) 25 grams, and nano silicon 50 grams, triethanolamine 5 grams mix subsequent use.120 ℃ solidified 1.5 hours.Coating layer thickness 20 nanometers.Carry out salt spray test, PCT test, damp heat test and high temperature demagnetize then and measure, can find out that the coating adhesion is good, cross cut test is qualified, and Corrosion Protection is referring to table 1.
Embodiment 2
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, nano ceramics is handled.Wherein main film forming agent is E-44 epoxy resin 25 grams, methyl ethyl ketone peroxide 15 grams, and nano aluminium oxide 65, diethanol amine 20 grams mix subsequent use.120 ℃ solidified 1.5 hours.Coating layer thickness 20 nanometers.The coating adhesion is good, and cross cut test is qualified, and Corrosion Protection is referring to table 1.
Embodiment 3
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, nano ceramics is handled.Wherein main film forming agent is E-51 epoxy resin 20 grams, methyl iso-butyl ketone (MIBK) 2 grams, and methyl ethyl ketone peroxide 20 grams, nano silicon 10 grams, aluminium oxide 50, triethanolamine 5 grams, diethanol amine 12 grams mix subsequent use.120 ℃ solidified 1.5 hours.Coating layer thickness 23 nanometers.Carry out salt spray test, PCT test, damp heat test and high temperature demagnetize then and measure, can find out that the coating adhesion is good, cross cut test is qualified, and Corrosion Protection is referring to table 1.
Embodiment 4
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, nano ceramics is handled.Wherein main film forming agent is E-44 epoxy resin 18 grams, methyl iso-butyl ketone (MIBK) 5 grams, methyl ethyl ketone peroxide 10 grams, peroxidating acetate uncle fourth fat 12 grams, and nano silicon 50 grams, aluminium oxide 10, diethanol amine 15 grams mix subsequent use.120 ℃ solidified 1.5 hours.Coating layer thickness 20 nanometers.Carry out salt spray test, PCT test, damp heat test and high temperature demagnetize then and measure, can find out that the coating adhesion is good, cross cut test is qualified, and Corrosion Protection is referring to table 1.
Embodiment 5
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, nano ceramics is handled.Wherein main film forming agent is E-44 epoxy resin 19 grams; Methyl iso-butyl ketone (MIBK), methyl ethyl ketone peroxide, peroxidating acetate uncle fourth fat were made into 24 by 1: 1: 1 and restrain; Nano silicon and aluminium oxide were made into 60 grams by 1: 3, and triethanolamine and diethanol amine were made into 15 grams by 1: 2 and mix subsequent use.120 ℃ solidified 1.5 hours.Coating layer thickness 20 nanometers.Carry out salt spray test, PCT test, damp heat test and high temperature demagnetize then and measure, can find out that the coating adhesion is good, cross cut test is qualified, and Corrosion Protection is referring to table 1.
Embodiment 6
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, nano ceramics is handled.Wherein main film forming agent is E-51 epoxy resin 15 grams, and methyl iso-butyl ketone (MIBK), methyl ethyl ketone peroxide, peroxidating acetate uncle fourth fat were made into 25 grams by 1: 2: 2, and nano silicon and aluminium oxide were made into 58 grams by 1: 1, and diethanol amine 13 grams mix subsequent use.120 ℃ solidified 1.5 hours.Coating layer thickness 20 nanometers.Carry out salt spray test, PCT test, damp heat test and high temperature demagnetize then and measure, can find out that the coating adhesion is good, cross cut test is qualified, and Corrosion Protection is referring to table 1.
The comparative example 1
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball-mill 2 hours.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after NaOH 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, table is transferred, and the utilization conventional method is carried out phosphatization.Carry out salt spray test, PCT test, damp heat test and high temperature demagnetize then and measure, Corrosion Protection is referring to table 1.(details consult Su Jiwen etc. publication number be the patent of 200510020633X).
Below, the experimental data of physical parameter is carried out in table 1 explanation through the coating that the foregoing description 1～6 is obtained.
Table 1
Can be found out that by table 1 coating surface of the present invention is even, corrosion resistance is high, and high temperature and pressure test and damp heat test (85 ℃ of temperature, humidity 80, relative humidity 100%) are compared with phosphatization with neutral salt spray test, and the present invention has good antiseptic effect.Simultaneously also can cost be reduced by 15～30%
Need to prove that the foregoing invention content and the specific embodiment are intended to prove the practical application of technical scheme provided by the present invention, should not be construed as qualification protection domain of the present invention.Those skilled in the art are in spirit of the present invention and principle, when doing various modifications, being equal to replacement or improvement.Protection scope of the present invention is as the criterion with appended claims.
Claims (10)
1. one kind is adopted nano ceramics that Nd-Fe-Bo permanent magnet material is carried out surface treatment method, and said method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: use sodium phosphate, sodium carbonate or NaOH that said Nd-Fe-Bo permanent magnet material is carried out conventional degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that said Nd-Fe-Bo permanent magnet material is carried out conventional acid pickling and rust removing, washing then;
(4) nano ceramics is handled: said Nd-Fe-Bo permanent magnet material is put into the nano ceramics plating bath carry out the nano ceramics processing, said nano ceramics plating bath comprises main film forming agent, coalescents, filler and curing agent; Wherein, Said main film forming agent is the epoxy resin that has amino or epoxy radicals; Said coalescents is selected from least a in methyl iso-butyl ketone (MIBK), methyl ethyl ketone peroxide and the peroxidating acetate uncle fourth fat; Said filler is nano silicon and/or aluminium oxide, and said curing agent is triethanolamine and/or diethanol amine; With
(5) wash, dry up, with the curing nano ceramic plated layer.
2. surface treatment method according to claim 1 is characterized in that, said main film forming agent is E-44 epoxy resin or E-51 epoxy resin.
3. surface treatment method according to claim 1 and 2 is characterized in that, the content of said main film forming agent is the 15-25 gram.
4. surface treatment method according to claim 1 is characterized in that, the content of said coalescents is the 15-25 gram.
5. surface treatment method according to claim 1 is characterized in that, the content of said filler is the 50-65 gram.
6. surface treatment method according to claim 1 is characterized in that, the content of said curing agent is the 5-20 gram.
7. surface treatment method according to claim 1 is characterized in that, said nano ceramics is handled and carried out at normal temperatures.
8. surface treatment method according to claim 1 is characterized in that, solidification temperature is 120 ℃, and be 1.5 hours hardening time.
9. surface treatment method according to claim 1 is characterized in that, the thickness of said nano ceramics coating is 20～23 nanometers.
10. surface treatment method according to claim 1 is characterized in that, said Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103938241A (en) * | 2014-04-08 | 2014-07-23 | 湖北桑夏太阳能产业有限公司 | Method for enhancing corrosion resistance of NdFeB (Neodymium Iron Boron) permanent magnet |
| CN107118380A (en) * | 2017-06-28 | 2017-09-01 | 昆山特酷信息科技有限公司 | A kind of preparation method of the hard plastics display screen of tablet personal computer |
| CN107151387A (en) * | 2017-06-28 | 2017-09-12 | 昆山特酷信息科技有限公司 | A kind of hard plastics display screen of tablet personal computer |
| CN107377330A (en) * | 2017-06-19 | 2017-11-24 | 苏州乔纳森新材料科技有限公司 | A kind of method that nano ceramics is surface-treated to Nd-Fe-B permanent magnet material |
| EP3967407A1 (en) | 2020-09-07 | 2022-03-16 | Yantai Shougang Magnetic Materials Inc. | A preparation device and method of ceramic coating on a sintered type ndfeb permanent magnet |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103938241A (en) * | 2014-04-08 | 2014-07-23 | 湖北桑夏太阳能产业有限公司 | Method for enhancing corrosion resistance of NdFeB (Neodymium Iron Boron) permanent magnet |
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| CN107377330A (en) * | 2017-06-19 | 2017-11-24 | 苏州乔纳森新材料科技有限公司 | A kind of method that nano ceramics is surface-treated to Nd-Fe-B permanent magnet material |
| CN107118380A (en) * | 2017-06-28 | 2017-09-01 | 昆山特酷信息科技有限公司 | A kind of preparation method of the hard plastics display screen of tablet personal computer |
| CN107151387A (en) * | 2017-06-28 | 2017-09-12 | 昆山特酷信息科技有限公司 | A kind of hard plastics display screen of tablet personal computer |
| EP3967407A1 (en) | 2020-09-07 | 2022-03-16 | Yantai Shougang Magnetic Materials Inc. | A preparation device and method of ceramic coating on a sintered type ndfeb permanent magnet |
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