CN102453890A - Zirconate surface treatment technology of permanent magnet - Google Patents
Zirconate surface treatment technology of permanent magnet Download PDFInfo
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- CN102453890A CN102453890A CN2010105146938A CN201010514693A CN102453890A CN 102453890 A CN102453890 A CN 102453890A CN 2010105146938 A CN2010105146938 A CN 2010105146938A CN 201010514693 A CN201010514693 A CN 201010514693A CN 102453890 A CN102453890 A CN 102453890A
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- surface treatment
- treatment method
- fluozirconate
- degreasing
- permanent magnet
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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- Chemical Treatment Of Metals (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention provides a zirconate surface treatment method of a permanent magnet. The method comprises steps of: (1) chamfering and polishing are carried out, wherein regular polishing is carried out upon a neodymium-iron-boron permanent magnetic material with a mechanical vibration grinding method and a barrel chamfering method; (2) degreasing and oil removing are carried out, wherein sodium phosphate, sodium carbonate or sodium hydroxide is added for carrying out regular degreasing and oil removing; (3) pickling and rust removing are carried out, wherein a nitric acid solution is added for carrying our regular pickling and rust removing, and the permanent magnetic material is washed by using water; (4) zirconate surface treatment is carried out by using a main film forming agent and a film forming auxiliary agent; and (5) the permanent magnetic material is washed and dried by blowing, such that the coating is cured. The adopted main film forming agent is silane-modified epoxy resin, and the film forming auxiliary agent is fluozirconate and/or fluorozirconic acid. The technology provided by the invention is advantaged in simple treatment, high speed, environment friendliness, and high corrosion resistance.
Description
Technical field
The present invention relates to the field of surface treatment of material, especially relate to the process for treating surface of Nd-Fe-Bo permanent magnet material, specifically, the present invention relates to a kind of zirconate sufacing that is used for permanent magnet material.
Background technology
Application of neodymium iron boron (NdFeB) permanent magnet material in recent years and development very rapidly, and the protection success or not of Nd-Fe-Bo permanent magnet material is related to one of gordian technique that can material apply.This material mainly is to be prepared from through powder metallurgical technique elements such as rare earth metal neodymium Nd, iron and boron.As the strongest present magneticsubstance, be widely used in all fields such as electroplating device, machinery, medical treatment, automobile, 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 the porous material that a kind of powder metallurgical technique is prepared from, because of rich neodymium phase wherein, neodymium iron boron principal phase and borderline phase are easy to form intergranular corrosion.Rear earth element nd in the neodymium iron boron powder alloy; Character is active; Make the corrosion resisting property of whole Nd-Fe-B alloys become very poor, very easily corrosion in damp and hot environment causes the decline or the damage of magnetic property because of corrosion failure; Have a strong impact on the work-ing life of Nd-Fe-B permanent magnet, reduced the stability and the safety of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its weave construction have very big relation.The principal phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property.To coercive force contribution maximum is rich neodymium phase.Huge variation will take place in the magnetic property of material after corrosion takes place Nd-Fe-Bo permanent magnet material.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.
The anti-corrosion method of Nd-Fe-Bo permanent magnet material has much at present.Electronickelling, electro-galvanizing (CN1421547A, CN1056133A) are wherein arranged, electroplate MULTI-LAYER NICKEL, copper facing (CN1514889A), several different methods such as phosphatization (200510020633X), electrocoating paint.
Summary of the invention
The objective of the invention is to overcome above-mentioned defective, a kind of zirconate surface treatment method of permanent magnet material is provided, improve the antiseptic property of permanent magnet material.Said zirconate surface treatment method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: add sodium phosphate, yellow soda ash or sodium hydroxide and carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: add salpeter solution again and carry out conventional acid pickling and rust removing, washing;
(4) adopt main membrane-forming agent and film coalescence aid to carry out the zirconate surface treatment; With
(5) wash, dry up, with solidified coating;
Wherein, said main membrane-forming agent is the improved epoxy resin of silane, and said film coalescence aid is fluozirconate and/or fluorine zirconic acid.
Preferably, the improved epoxy resin of said silane is Si (OC
2H
5)
3The E-51 epoxy resin of modification or Si (OCH
3)
3The E-44 epoxy resin of modification.
Preferably, said fluozirconate is sodium fluozirconate or potassium fluozirconate.
Preferably, the content of said main membrane-forming agent is at 15～25 grams.The content of said film coalescence aid is 15～25 grams.
Preferably, the fluozirconate surface treatment is to carry out at normal temperatures.
Preferably, the thickness of said coating is 15～20 nanometers.
Preferably, said permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
The present invention handles simply, environmental protection fast, the performance that solidity to corrosion is high.The zirconate surface treatment is to be that main raw material carries out surface treatment to sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material with improved epoxy resin of silane and zirconate, and is not phosphorous, need not to heat.Treating processes does not produce sediment, and the treatment time is short, controls easy.Treatment step is few, can save table and transfer operation, and tank liquor is reusable.Effectively improve the sticking power of paint to base material.Coating is normal temperature solidified, also can dry film forming, has filled up a blank of domestic permanent magnetic material surface treatment industry.
Embodiment
Below will combine embodiment that the present invention is further specified, embodiments of the invention only are 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, zirconate surface treatment.Wherein main membrane-forming agent is for utilizing Si (OC
2H
5)
3E-51 epoxy resin 15 gram of modification, fluorine zirconic acid 5 grams, sodium fluozirconate 10 grams add be made into 1 liter subsequent use.Coat-thickness 20 nanometers, the coating bonding force is good, and cross cut test is qualified, carries out salt-fog test, humid heat test and high temperature demagnetize then and measures, 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, zirconate surface treatment.Wherein main membrane-forming agent is for utilizing Si (OCH
3)
3E-44 epoxy resin 25 gram of modification, fluorine zirconic acid 10 grams, potassium fluozirconate 15 grams add be made into 1 liter subsequent use.Coat-thickness 15 nanometers, the coating bonding force is good, and cross cut test is qualified, carries out salt-fog test, humid heat test and high temperature demagnetize then and measures, 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, zirconate surface treatment.Wherein main membrane-forming agent is for utilizing Si (OC
2H
5)
3E-51 epoxy resin 18 gram of modification, fluorine zirconic acid 15 grams, sodium fluozirconate 10 grams add be made into 1 liter subsequent use.Coat-thickness 20 nanometers, the coating bonding force is good, and cross cut test is qualified, carries out salt-fog test, humid heat test and high temperature demagnetize then and measures, 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, zirconate surface treatment.Wherein main membrane-forming agent is for utilizing Si (OC
2H
5)
3E-51 epoxy resin 19 gram of modification, fluorine zirconic acid 15 grams, sodium fluozirconate 10 grams add be made into 1 liter subsequent use.Coat-thickness 20 nanometers, the coating bonding force is good, and cross cut test is qualified, carries out salt-fog test, humid heat test and high temperature demagnetize then and measures, 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, zirconate surface treatment.Wherein main membrane-forming agent is for utilizing Si (OC
2H
5)
3E-51 epoxy resin 15 gram of modification, fluorine zirconic acid 5 grams, sodium fluozirconate 10 grams add be made into 1 liter subsequent use.Coat-thickness 20 nanometers, the coating bonding force is good, and cross cut test is qualified, carries out salt-fog test, humid heat test and high temperature demagnetize then and measures, 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, zirconate surface treatment.Wherein main membrane-forming agent is for utilizing Si (OC
2H
5)
3E-51 epoxy resin 15 gram of modification, fluorine zirconic acid 5 grams, sodium fluozirconate 10 grams add be made into 1 liter subsequent use.Coat-thickness 20 nanometers.The coating bonding force is good, and cross cut test is qualified, carries out salt-fog test, humid heat test and high temperature demagnetize then and measures, 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 ￠ 24* ￠ 15*18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washing, table is transferred, and the utilization ordinary method is carried out phosphatization.The coating bonding force is good, and cross cut test is qualified, and 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 find out by table 1; Coatingsurface of the present invention is even, and solidity to corrosion is high, high temperature and pressure test (hour) and humid heat test (85 ℃ of temperature, humidity 80; Relative humidity 100%) compare with comparative example 1 phosphatization with neutral salt spray test, have good preservative effect.Simultaneously also can cost be reduced by 15～30%
Need to prove that foregoing invention content and 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 (8)
1. the zirconate surface treatment method of a permanent magnet material, said surface treatment method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration, barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: add sodium phosphate, yellow soda ash or sodium hydroxide and carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: add salpeter solution again and carry out conventional acid pickling and rust removing, washing;
(4) adopt main membrane-forming agent and film coalescence aid to carry out the zirconate surface treatment; With
(5) wash, dry up, with solidified coating;
Wherein, said main membrane-forming agent is the improved epoxy resin of silane, and said film coalescence aid is fluozirconate and fluorine zirconic acid.
2. surface treatment method as claimed in claim 1, wherein, the improved epoxy resin of said silane is Si (OC
2H
5)
3The E-51 epoxy resin of modification or Si (OCH
3)
3The E-44 epoxy resin of modification.
3. surface treatment method as claimed in claim 1, wherein, said fluozirconate is sodium fluozirconate or potassium fluozirconate;
4. surface treatment method as claimed in claim 1, wherein, the content of said main membrane-forming agent is at 15～25 grams.
5. surface treatment method as claimed in claim 1, wherein, the content of said film coalescence aid is 15～25 grams.
6. like claim 1 or 3 described surface treatment methods, wherein, the fluozirconate surface treatment is to carry out at normal temperatures.
7. surface treatment method as claimed in claim 1, wherein, the thickness of said coating is 15～20 nanometers.
8. surface treatment method as claimed in claim 1, wherein, said permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010514693.8A CN102453890B (en) | 2010-10-14 | 2010-10-14 | A kind of zirconate process for treating surface of permanent magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010514693.8A CN102453890B (en) | 2010-10-14 | 2010-10-14 | A kind of zirconate process for treating surface of permanent magnet |
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| Publication Number | Publication Date |
|---|---|
| CN102453890A true CN102453890A (en) | 2012-05-16 |
| CN102453890B CN102453890B (en) | 2015-11-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010514693.8A Active CN102453890B (en) | 2010-10-14 | 2010-10-14 | A kind of zirconate process for treating surface of permanent magnet |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805798A (en) * | 2017-10-23 | 2018-03-16 | 杭州五源科技实业有限公司 | Graphene prefilming agent and its preparation and application before coated metal |
| CN115584496A (en) * | 2022-10-25 | 2023-01-10 | 福建省长汀金龙稀土有限公司 | Surface treatment method for permanent magnet, permanent magnet and protective film thereof |
Citations (4)
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|---|---|---|---|---|
| CN1702139A (en) * | 2004-05-25 | 2005-11-30 | 上海赛科现代交通设备有限公司 | Epoxy sealing material for linear motor stator electric magnet |
| CN101724830A (en) * | 2008-10-16 | 2010-06-09 | 北京中科三环高技术股份有限公司 | Nickel plating bath for permanent magnet material and permanent magnet material surface treatment method thereof |
| CN101728042A (en) * | 2008-10-16 | 2010-06-09 | 北京中科三环高技术股份有限公司 | Technique for treating surface of permanent magnet material |
| CN101728043A (en) * | 2008-10-16 | 2010-06-09 | 北京中科三环高技术股份有限公司 | Permanent magnet with corrosion resistant coating and powder nanometer spraying method thereof |
-
2010
- 2010-10-14 CN CN201010514693.8A patent/CN102453890B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1702139A (en) * | 2004-05-25 | 2005-11-30 | 上海赛科现代交通设备有限公司 | Epoxy sealing material for linear motor stator electric magnet |
| CN101724830A (en) * | 2008-10-16 | 2010-06-09 | 北京中科三环高技术股份有限公司 | Nickel plating bath for permanent magnet material and permanent magnet material surface treatment method thereof |
| CN101728042A (en) * | 2008-10-16 | 2010-06-09 | 北京中科三环高技术股份有限公司 | Technique for treating surface of permanent magnet material |
| CN101728043A (en) * | 2008-10-16 | 2010-06-09 | 北京中科三环高技术股份有限公司 | Permanent magnet with corrosion resistant coating and powder nanometer spraying method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805798A (en) * | 2017-10-23 | 2018-03-16 | 杭州五源科技实业有限公司 | Graphene prefilming agent and its preparation and application before coated metal |
| CN115584496A (en) * | 2022-10-25 | 2023-01-10 | 福建省长汀金龙稀土有限公司 | Surface treatment method for permanent magnet, permanent magnet and protective film thereof |
| WO2024087548A1 (en) * | 2022-10-25 | 2024-05-02 | 福建省金龙稀土股份有限公司 | Surface treatment method for permanent magnet, permanent magnet and protective film thereof |
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| CN102453890B (en) | 2015-11-25 |
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