CN107116211A - NdFeB magnetic powder surface oxidation-resistant processing method - Google Patents
NdFeB magnetic powder surface oxidation-resistant processing method Download PDFInfo
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- CN107116211A CN107116211A CN201710167798.2A CN201710167798A CN107116211A CN 107116211 A CN107116211 A CN 107116211A CN 201710167798 A CN201710167798 A CN 201710167798A CN 107116211 A CN107116211 A CN 107116211A
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- Prior art keywords
- magnetic powder
- spray evaporation
- ndfeb magnetic
- ndfeb
- solution
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 58
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 51
- 238000010301 surface-oxidation reaction Methods 0.000 title claims abstract description 18
- 238000003672 processing method Methods 0.000 title claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 40
- 230000008020 evaporation Effects 0.000 claims abstract description 40
- 239000007921 spray Substances 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 5
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 claims abstract description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 abstract description 15
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002131 composite material Substances 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Hard Magnetic Materials (AREA)
- Soft Magnetic Materials (AREA)
Abstract
This application discloses a kind of NdFeB magnetic powder surface oxidation-resistant processing method, including step：(1) pre-oxidation treatment, is carried out to NdFeB magnetic powder using spray evaporation mode, spray evaporation solution is 1~2wt.% of mass concentration dichromate solutions, the mixed liquor of mass concentration 3~5wt.% phosphoric acid solutions；(2) after-treatment, is carried out to the NdFeB magnetic powder of pre-oxidation using spray evaporation mode, spray evaporation solution is 1~5wt.% solution of sodium bisulfite；(3), NdFeB magnetic powder is post-processed using spray evaporation mode, spray evaporation solution is sodium hydroxide solution；(4), dry, obtaining surface has the ultra-fine NdFeB permanet magnetic powder of fine and close oxygen-proof film.The present invention realizes efficiently quickly magnetic surface modification processing using spray evaporation device, the composite membrane of formation is comparatively dense and uniform, the burr and corner angle of super-fine magnetic powder are eliminated by preoxidation process, the mobility and apparent density of neodymium iron boron super-fine magnetic powder are added, the inoxidizability of neodymium iron boron super-fine magnetic powder is improved.
Description
Technical field
The application is related to the process of surface treatment of magnetic material, at more particularly to a kind of NdFeB magnetic powder surface oxidation-resistant
Reason method.
Background technology
The characteristics of nd-fe-b permanent magnetic alloy powder is:Magnetic property is good, and mechanical property is good, but Curie temperature Tc is low, temperature stabilization
Property is poor, and chemical inoxidizability is not good, therefore limits its application.The premise of iron B permanent magnetic material application is to first have to solution
Certainly anti-oxidation, the Anticorrosion of good material.Rare earth element particularly in Nd Fe B alloys powder, property is active, makes whole neodymium
The antioxygenic property of iron boron magnetic powder becomes very poor, the easily oxidation and rusting in damp and hot environment.In addition, Nd-Fe-B permanent magnet material
Magnetic property has very big relation with its institutional framework, and the principal phase of Nd-Fe-B permanent magnet is the main source of magnet magnetic property, wherein,
Contribute maximum to coercivity is rich neodymium phase.After Nd-Fe-B permanent magnet material is aoxidized, the magnetic property of material will occur huge
Big change.The decline or damage of Nd-Fe-B permanent magnet magnetic property caused by oxidation peeling failure, have had a strong impact on neodymium iron boron forever
The service life of magnet, reduces the stability and reliability of product.Therefore, the inoxidizability problem one of Nd-Fe-B permanent magnet material
It is directly the subject matter that Nd-Fe-B permanent magnet material needs to solve.At present, anti-oxidant, the anti-corrosion method of Nd-Fe-B permanent magnet material have very
It is many.Wherein there are galvanoplastic (CN1421547A), phosphorization filming method (A of CN 105803443), surface is modified organic coated method (CN
105788793 A), a variety of methods such as preoxidation (A of CN 105478787).But, wherein galvanoplastic cost is higher, environment
Pollution is big.Although traditional Nd-Fe-B permanent magnetic super-fine magnetic powder surface oxidation-resistant method effect is preferably, inefficiency, it is more difficult to control table
Face modification process.
The content of the invention
It is an object of the invention to provide a kind of NdFeB magnetic powder surface oxidation-resistant processing method, to overcome in the prior art
Deficiency.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of NdFeB magnetic powder surface oxidation-resistant processing method, including step：
(1) pre-oxidation treatment, is carried out to NdFeB magnetic powder using spray evaporation mode, spray evaporation solution is mass concentration
The mixed liquor of 1~2wt.% dichromate solutions, mass concentration 3~5wt.% phosphoric acid solutions；
(2) after-treatment, is carried out to the NdFeB magnetic powder of pre-oxidation using spray evaporation mode, spray evaporation solution is 1
~5wt.% solution of sodium bisulfite；
(3), NdFeB magnetic powder is post-processed using spray evaporation mode, spray evaporation solution is that sodium hydroxide is molten
Liquid；
(4), dry, obtaining surface has the ultra-fine NdFeB permanet magnetic powder of fine and close oxygen-proof film.
It is preferred that, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (1), spray evaporation
During, the environment temperature for controlling NdFeB magnetic powder is 50 DEG C -60 DEG C, relative humidity 50%-80%.
It is preferred that, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (2), spray evaporation
During, pH=9~10 of moisture are controlled by adjusting evaporation rate, the environment temperature for controlling NdFeB magnetic powder is 50~60
DEG C, relative humidity 60~80%.
It is preferred that, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (4), drying temperature
For 80~90 DEG C, drying time is 25~45min.
It is preferred that, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, in the step (1) and step (2),
NdFeB magnetic powder is tiled on a moving belt with certain thickness and passes through spray evaporation room with 0.3~0.5m/min.
It is preferred that, in above-mentioned NdFeB magnetic powder surface oxidation-resistant processing method, NdFeB magnetic powder is flat with 1-2mm thickness
Paving is on a moving belt.
Compared with prior art, the advantage of the invention is that：The present invention is realized efficiently quick using spray evaporation device
The processing of magnetic surface modification, the composite membrane of formation is comparatively dense and uniform, and super-fine magnetic powder is eliminated by preoxidation process
Burr and corner angle, add the mobility and apparent density of neodymium iron boron super-fine magnetic powder, improve the antioxygen of neodymium iron boron super-fine magnetic powder
The property changed.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
Embodiment 1
Nd-Fe-B permanent magnetic 10um or so superfine powder is tiled on a moving belt with 1mm thickness, and with 0.5m/min by spraying
Vaporization chamber, oxidizing temperature is 60 DEG C, relative humidity 80%, and spray evaporation solution is composite solution, and solution includes mass concentration
2wt.% dichromate solutions and mass concentration 3wt.% phosphoric acid solutions；Gained pre-oxidation neodymium iron boron super-fine magnetic powder again with
The tiling of 1mm thickness passes through spray evaporation room with 0.5m/min on a moving belt, now, and the solution of spray evaporation is 1~5wt.%
Solution of sodium bisulfite, and evaporation chamber outlet end increase a spray evaporator by sodium hydroxide solution spray evaporation, lead to
The PH=9 that evaporation rate controls moisture is overregulated, temperature is 50 DEG C, relative humidity 80%；Last neodymium iron boron super-fine magnetic powder passes through
Dried in conveyer belt feeding drying chamber, drying temperature is 90 DEG C, drying time is 25min, next step vibration sub-sieve will meet grain
Degree requires and is that dry powder is fallen into collector, produces the ultra-fine NdFeB permanet magnetic powder with fine and close oxygen-proof film.
Embodiment 2
Nd-Fe-B permanent magnetic 20-40um or so fine powder is tiled on a moving belt with 1.5mm thickness, and with 0.4m/min by spraying
Mist vaporization chamber, oxidizing temperature is 60 DEG C, relative humidity 80%, and spray evaporation solution is composite solution, and solution includes mass concentration
1wt.% dichromate solution quality and quantity concentration 4wt.% phosphoric acid solutions；Gained pre-oxidation neodymium iron boron super-fine magnetic powder again with
The tiling of 1mm thickness passes through spray evaporation room with 0.5m/min on a moving belt, now, and the solution of spray evaporation is a certain amount of sulfurous
Sour hydrogen sodium solution, and increase a spray evaporator by sodium hydroxide solution spray evaporation in evaporation chamber outlet end, pass through regulation
Evaporation rate controls the PH=10 of moisture, and temperature is 60 DEG C, relative humidity 70%；Last neodymium iron boron super-fine magnetic powder passes through conveyer belt
Send into drying chamber and dry, drying temperature is 80 DEG C, drying time is 30min, next step vibration sub-sieve will meet granularity requirements
And be that dry powder is fallen into collector, produce the ultra-fine NdFeB permanet magnetic powder with fine and close oxygen-proof film.
Finally, in addition it is also necessary to explanation, term " comprising ", "comprising" or its any other variant are intended to non-exclusive
Property include so that process, method, article or equipment including a series of key elements not only include those key elements, and
Also include other key elements for being not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (6)
1. a kind of NdFeB magnetic powder surface oxidation-resistant processing method, it is characterised in that including step：
(1), using spray evaporation mode to NdFeB magnetic powder carry out pre-oxidation treatment, spray evaporation solution be mass concentration 1~
The mixed liquor of 2wt.% dichromate solutions, mass concentration 3~5wt.% phosphoric acid solutions；
(2) after-treatment, is carried out to the NdFeB magnetic powder of pre-oxidation using spray evaporation mode, spray evaporation solution is 1~
5wt.% solution of sodium bisulfite；
(3), NdFeB magnetic powder is post-processed using spray evaporation mode, spray evaporation solution is sodium hydroxide solution；
(4), dry, obtaining surface has the ultra-fine NdFeB permanet magnetic powder of fine and close oxygen-proof film.
2. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that：The step (1)
In, during spray evaporation, the environment temperature for controlling NdFeB magnetic powder is 50 DEG C -60 DEG C, relative humidity 50%-80%.
3. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that：The step (2)
In, during spray evaporation, pH=9~10 of moisture are controlled by adjusting evaporation rate, the environment temperature of NdFeB magnetic powder is controlled
Spend for 50~60 DEG C, relative humidity 60~80%.
4. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that：The step (4)
In, drying temperature is 80~90 DEG C, and drying time is 25~45min.
5. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 1, it is characterised in that：The step (1)
In step (2), NdFeB magnetic powder is tiled on a moving belt with certain thickness and passes through spray evaporation with 0.3~0.5m/min
Room.
6. NdFeB magnetic powder surface oxidation-resistant processing method according to claim 5, it is characterised in that：NdFeB magnetic powder with
1-2mm thickness tiles on a moving belt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710167798.2A CN107116211B (en) | 2017-03-21 | 2017-03-21 | NdFeB magnetic powder surface oxidation-resistant processing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710167798.2A CN107116211B (en) | 2017-03-21 | 2017-03-21 | NdFeB magnetic powder surface oxidation-resistant processing method |
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| Publication Number | Publication Date |
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| CN107116211A true CN107116211A (en) | 2017-09-01 |
| CN107116211B CN107116211B (en) | 2019-03-12 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362681A (en) * | 2019-12-11 | 2020-07-03 | 横店集团东磁股份有限公司 | High-performance permanent magnetic ferrite magnet sintered after injection molding and preparation method thereof |
| CN111370198A (en) * | 2019-12-20 | 2020-07-03 | 横店集团东磁股份有限公司 | Injection-molded soft magnetic ferrite magnet and preparation method thereof |
| CN111370216A (en) * | 2020-03-12 | 2020-07-03 | 江苏巨鑫磁业有限公司 | Oxidation resisting method for omnibearing film attachment on surface of magnetic powder particles |
| CN114101687A (en) * | 2021-12-07 | 2022-03-01 | 鞍山安特磁材有限公司 | Novel pressure-resistant magnetic powder |
| CN116511497A (en) * | 2023-03-23 | 2023-08-01 | 江苏巨鑫磁业有限公司 | Magnetic powder surface antioxidation processing device |
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|---|---|---|---|---|
| CN1085963A (en) * | 1993-11-03 | 1994-04-27 | 胡景云 | The swimming of neodymium-iron-boron magnetic material cathode of surface applies production technique |
| CN1528952A (en) * | 2003-09-27 | 2004-09-15 | 沈阳工业学院 | Neodymium-iron-boron magnet zinc plating and cathode electrophoresis composite protection process |
| JP2009185340A (en) * | 2008-02-07 | 2009-08-20 | Tayca Corp | Metallic powder having insulation film formed thereon by using peelable double hydroxide and production method therefor |
| CN102464902A (en) * | 2010-11-16 | 2012-05-23 | 北京中科三环高技术股份有限公司 | Surface treating method of Cr-Zn coating of Nd-Fe-B permanent magnet material |
| CN105478787A (en) * | 2015-12-03 | 2016-04-13 | 江苏巨鑫磁业有限公司 | Oxidization method of rapidly-quenched bonded neodymium iron boron (NdFeB) permanent magnet powder |
-
2017
- 2017-03-21 CN CN201710167798.2A patent/CN107116211B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085963A (en) * | 1993-11-03 | 1994-04-27 | 胡景云 | The swimming of neodymium-iron-boron magnetic material cathode of surface applies production technique |
| CN1528952A (en) * | 2003-09-27 | 2004-09-15 | 沈阳工业学院 | Neodymium-iron-boron magnet zinc plating and cathode electrophoresis composite protection process |
| JP2009185340A (en) * | 2008-02-07 | 2009-08-20 | Tayca Corp | Metallic powder having insulation film formed thereon by using peelable double hydroxide and production method therefor |
| CN102464902A (en) * | 2010-11-16 | 2012-05-23 | 北京中科三环高技术股份有限公司 | Surface treating method of Cr-Zn coating of Nd-Fe-B permanent magnet material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362681A (en) * | 2019-12-11 | 2020-07-03 | 横店集团东磁股份有限公司 | High-performance permanent magnetic ferrite magnet sintered after injection molding and preparation method thereof |
| CN111370198A (en) * | 2019-12-20 | 2020-07-03 | 横店集团东磁股份有限公司 | Injection-molded soft magnetic ferrite magnet and preparation method thereof |
| CN111370216A (en) * | 2020-03-12 | 2020-07-03 | 江苏巨鑫磁业有限公司 | Oxidation resisting method for omnibearing film attachment on surface of magnetic powder particles |
| CN114101687A (en) * | 2021-12-07 | 2022-03-01 | 鞍山安特磁材有限公司 | Novel pressure-resistant magnetic powder |
| CN116511497A (en) * | 2023-03-23 | 2023-08-01 | 江苏巨鑫磁业有限公司 | Magnetic powder surface antioxidation processing device |
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| CN107116211B (en) | 2019-03-12 |
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