CN104342614A - Surface treatment method of chemical protection layer of sintered neodymium iron boron permanent magnet material for automobile - Google Patents
Surface treatment method of chemical protection layer of sintered neodymium iron boron permanent magnet material for automobile Download PDFInfo
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- CN104342614A CN104342614A CN201310342741.3A CN201310342741A CN104342614A CN 104342614 A CN104342614 A CN 104342614A CN 201310342741 A CN201310342741 A CN 201310342741A CN 104342614 A CN104342614 A CN 104342614A
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- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
- C23C8/18—Oxidising of ferrous surfaces
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/026—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention provides a surface treatment method of a chemical protection layer of a sintered neodymium iron boron permanent magnet material for an automobile. The surface treatment method comprises the following steps of: (1) degreasing and removing oil: adding sodium phosphate, sodium carbonate and sodium hydroxide for conventional degreasing and oil removal of the polished permanent magnet material, and blowdrying, and (2) forming a ferroferric oxide protection layer on the surface of the neodymium iron boron permanent magnet by a barffing method, wherein the ferroferric oxide protection layer is obtained by supplying water vapor after the degreased, deoiled and blowdried neodymium iron boron permanent magnet material is heated in a furnace at 300-350 DEG C for 10min, and carrying out heat treatment reaction at 250-450 DEG C when the air pressure of the water vapor is at 0.05-600Pa. The protection layer prepared by the method has the advantages of good coating binding force and high corrosion resistance.
Description
Technical field
The present invention relates to the field of surface treatment of material, especially relate to the surface treatment method of automobile sintered Nd-Fe-B permanent magnetic material chemical protection layer.
Background technology
The application and development of neodymium iron boron (NdFeB) permanent magnet material is very rapid in recent years, 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 is mainly prepared from by powder metallurgical technique by elements such as rare earth metal neodymium Nd, iron and boron.As magneticsubstance the strongest at present, be widely used in all fields such as electroplating device, machinery, medical treatment, automobile, application prospect is very wide.
The prerequisite of Nd-Fe-Bo permanent magnet material application first to resolve the Anticorrosion 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 border are easy to form intergranular corrosion mutually.Rear earth element nd in neodymium iron boron powder metallurgy, character is active, the corrosion resisting property of whole Nd-Fe-B alloys is made to become very poor, very easily corrosion in damp and hot environment, because corrosion failure causes decline or the damage of magnetic property, have a strong impact on the work-ing life of Nd-Fe-B permanent magnet, reduce stability and the reliability of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its weave construction have very large relation.The principal phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property.Maximum to coercive force contribution is rich neodymium phase.To there is huge change in the magnetic property of material after corrosion occurs Nd-Fe-Bo permanent magnet material.Therefore, the Anticorrosion of Nd-Fe-Bo permanent magnet material is the subject matter that Nd-Fe-Bo permanent magnet material needs to solve always.
The anti-corrosion method of current Nd-Fe-Bo permanent magnet material has a lot.Wherein there are electronickelling, electro-galvanizing (CN1421547A, CN1056133A), shooting of multi-layer nickel electroplating, copper facing (CN1514889A), the multiple method such as phosphatization, electrocoating paint, passivation.And wherein passivation is applied for a patent a lot, wherein Hitachi Metals Zhu Shi commercial firm has applied for 5 sections of (CN200980125595, CN200980134446, CN200880109023, CN201080062182, CN201180032708) Patents.
Even if wherein CN200880109023 provides a kind of in the environment of humidity variation, the rare-earth sintered magnet of sufficient corrosion-resistant system also can be given by oxidizing thermal treatment.The method is 1 × 102Pa ~ 1 × 105Pa in oxygen partial pressure, under steam partial pressure is the atmosphere of 0.1Pa ~ 1000Pa (but except 1000Pa), in 200 DEG C ~ 600 DEG C magnet body is heat-treated to obtain a kind of be main oxide film by rhombohedral iron ore.
Even if CN201180032708 problem of the present invention is to provide a kind of corrosion stability also in the environment of temperature and humidity variation with extremely excellence, and has the manufacture method of the rare-earth sintered magnet through surface modification of excellent magnetic properties.As the manufacture method of the rare-earth sintered magnet through surface modification of the present invention of its solution, it is characterized in that, comprise to rare-earth sintered magnet oxygen partial pressure be 1 × 103Pa ~ 1 × 105Pa, steam partial pressure is below 45Pa, and the ratio of oxygen partial pressure and steam partial pressure (oxygen partial pressure/steam partial pressure) is under the atmosphere of 450 ~ 20000,200 DEG C ~ 600 DEG C operations of heat-treating.
But the high-temperature water vapor process of ironware mainly adopts under differing temps and vapor pressure, can generate three kinds of oxide compounds, ferric oxide, iron protoxide and Z 250, and iron protoxide and ferric oxide are a kind of very loose oxide compounds.Contrary Z 250 is a kind of hard anodic oxidation coating, is the oxide compound obtained desired by steam treatment.
Summary of the invention
The object of the invention is to overcome above-mentioned defect, provide a kind of surface treatment method of automobile sintered Nd-Fe-B permanent magnetic material chemical protection layer, to improve the antiseptic property of permanent magnet material.
According to the surface treatment method of automobile sintered Nd-Fe-B permanent magnetic material chemical protection layer of the present invention, described surface treatment method comprises the steps: (1) degreasing degreasing: add sodium phosphate, sodium carbonate and sodium hydroxide and grinded permanent magnet material is carried out to conventional degreasing degreasing, dries up; (2) method of barffing is adopted to form a kind of protective layer by Z 250 at surface of Nd-Fe-B permanent magnet; Wherein, by through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 300-350 DEG C of preheating and pass into water vapor after 10 minutes, vapor pressure of water 0.05Pa ~ 600Pa heat-treats at 250 DEG C ~ 450 DEG C and is obtained by reacting a kind of protective layer by Z 250.
Preferably, the time of heat-treating reaction at 250-450 DEG C is 0.5-3 hour.
Preferably, the thickness 0.2-10 micron of described protective layer.
By the protective layer that method of the present invention is obtained, there is binding force of cladding material good, the advantage that antiseptic property is high.
Embodiment
Below with reference to embodiment, the present invention will be further described, and embodiments of the invention are only for illustration of technical scheme of the present invention, and non-limiting the present invention.
Embodiment 1
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 300 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 0.05Pa is within 0.5 hour, obtain a kind of protective layer by Z 250 in the time that 250 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 0.2 micron.Refer to table 1.
Embodiment 2
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 350 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 600Pa is within 3 hours, obtain a kind of protective layer by Z 250 in the time that 450 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 10 microns.Refer to table 1.
Embodiment 3
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 320 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 50Pa is within 0.5 hour, obtain a kind of protective layer by Z 250 in the time that 400 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 0.5 micron.Refer to table 1.
Embodiment 4
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 300 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 100Pa is within 2 hours, obtain a kind of protective layer by Z 250 in the time that 280 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 1 micron.Refer to table 1.
Embodiment 5
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 320 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 15Pa is within 2 hours, obtain a kind of protective layer by Z 250 in the time that 420 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 2 microns.Refer to table 1.
Embodiment 6
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 330 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 150Pa is within 1.5 hours, obtain a kind of protective layer by Z 250 in the time that 350 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 3 microns.Refer to table 1.
Embodiment 7
Sintered Nd-Fe-B permanent magnetic material 2.3 kilograms of elder generations of 28*18*7mm are polished 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, dries up.By through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 320 DEG C of preheatings and pass into water vapor after 10 minutes, vapor pressure of water 320Pa is within 0.5 hour, obtain a kind of protective layer by Z 250 in the time that 380 DEG C are heat-treated reaction heat treatment reaction.The thickness of protective layer 0.5 micron.Refer to table 1.
Table 1
Embodiment | Salt Jin (5% sodium-chlor) (hour) | High temperature demagnetizing factor |
Embodiment 1 | 4 | 0.02 |
Embodiment 2 | 5 | 0.04 |
Embodiment 3 | 5 | 0.03 |
Embodiment 4 | 6 | 0.04 |
Embodiment 5 | 5 | 0.02 |
Embodiment 6 | 6 | 0.03 |
Embodiment 7 | 5 | 0.04 |
As can be seen from embodiments of the invention, the salt leaching of protective layer of the present invention was higher than 4 hours, and high temperature demagnetizing factor is similar to body material lower than 0.05%, and it is suitable with normal process to have good preservative effect.
It should be noted that, foregoing invention content and embodiment are intended to the practical application proving technical scheme provided by the present invention, should not be construed as limiting the scope of the present invention.Those skilled in the art in spirit of the present invention and principle, when doing various amendment, equivalent replace or improve.Protection scope of the present invention is as the criterion with appended claims.
Claims (3)
1. an automobile surface treatment method for sintered Nd-Fe-B permanent magnetic material chemical protection layer, described surface treatment method comprises the steps:
(1) degreasing degreasing: add sodium phosphate, sodium carbonate and sodium hydroxide and grinded permanent magnet material is carried out conventional degreasing degreasing, dried up; With
(2) method of barffing is adopted to form a kind of protective layer by Z 250 at surface of Nd-Fe-B permanent magnet; Wherein, by through degreasing degreasing and the Nd-Fe-Bo permanent magnet material dried up be placed in stove and be heated to 300-350 DEG C of preheating and pass into water vapor after 10 minutes, vapor pressure of water 0.05Pa ~ 600Pa heat-treats at 250 DEG C ~ 450 DEG C and is obtained by reacting a kind of protective layer by Z 250.
2. surface treatment method as claimed in claim 1, wherein, the time of heat-treating reaction at 250-450 DEG C is 0.5-3 hour.
3. surface treatment method as claimed in claim 1, wherein, the thickness 0.2-10 micron of described protective layer.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107464684A (en) * | 2017-08-30 | 2017-12-12 | 包头天和磁材技术有限责任公司 | The processing method of sintered magnet |
CN111755236A (en) * | 2020-06-23 | 2020-10-09 | 安泰科技股份有限公司 | Bluing anti-corrosion method for sintered neodymium-iron-boron magnet |
CN112746296A (en) * | 2019-12-02 | 2021-05-04 | 天津京磁电子元件制造有限公司 | Method for electroplating copper on neodymium iron boron magnet |
CN112768169A (en) * | 2020-12-30 | 2021-05-07 | 包头天和磁材科技股份有限公司 | Preform, method for producing the same, method for producing corrosion-resistant magnet, and use of the same |
CN113555208A (en) * | 2021-06-11 | 2021-10-26 | 杭州电子科技大学 | Surface treatment method of sintered neodymium-iron-boron magnet and sintered neodymium-iron-boron magnet |
CN113667970A (en) * | 2020-05-03 | 2021-11-19 | 江西金力永磁科技股份有限公司 | Surface passivation treatment method for neodymium iron boron magnetic steel |
CN117488235A (en) * | 2024-01-03 | 2024-02-02 | 张家港市港威超声电子有限公司 | Automatic bluing equipment of neodymium iron boron |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107464684A (en) * | 2017-08-30 | 2017-12-12 | 包头天和磁材技术有限责任公司 | The processing method of sintered magnet |
CN107464684B (en) * | 2017-08-30 | 2020-04-21 | 包头天和磁材科技股份有限公司 | Method for treating sintered magnet |
CN112746296A (en) * | 2019-12-02 | 2021-05-04 | 天津京磁电子元件制造有限公司 | Method for electroplating copper on neodymium iron boron magnet |
CN113667970A (en) * | 2020-05-03 | 2021-11-19 | 江西金力永磁科技股份有限公司 | Surface passivation treatment method for neodymium iron boron magnetic steel |
CN111755236A (en) * | 2020-06-23 | 2020-10-09 | 安泰科技股份有限公司 | Bluing anti-corrosion method for sintered neodymium-iron-boron magnet |
CN112768169A (en) * | 2020-12-30 | 2021-05-07 | 包头天和磁材科技股份有限公司 | Preform, method for producing the same, method for producing corrosion-resistant magnet, and use of the same |
CN113555208A (en) * | 2021-06-11 | 2021-10-26 | 杭州电子科技大学 | Surface treatment method of sintered neodymium-iron-boron magnet and sintered neodymium-iron-boron magnet |
CN113555208B (en) * | 2021-06-11 | 2023-11-10 | 杭州电子科技大学 | Surface treatment method of sintered NdFeB magnet and sintered NdFeB magnet |
CN117488235A (en) * | 2024-01-03 | 2024-02-02 | 张家港市港威超声电子有限公司 | Automatic bluing equipment of neodymium iron boron |
CN117488235B (en) * | 2024-01-03 | 2024-05-10 | 张家港市港威超声电子有限公司 | Automatic bluing equipment of neodymium iron boron |
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Application publication date: 20150211 |