CN110444385A - A kind of coercitive technique of promotion Nd-Fe-B magnet - Google Patents
A kind of coercitive technique of promotion Nd-Fe-B magnet Download PDFInfo
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- CN110444385A CN110444385A CN201910736073.XA CN201910736073A CN110444385A CN 110444385 A CN110444385 A CN 110444385A CN 201910736073 A CN201910736073 A CN 201910736073A CN 110444385 A CN110444385 A CN 110444385A
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- magnet
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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
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of coercitive techniques of promotion Nd-Fe-B magnet, after needing the magnet being sintered to be cut into the shape of needs, carry out pickling pretreatment；It carries out inhaling hydrogen processing, the suction hydrogen process of magnet is carried out in the container with extraction gas for being connected with recirculated water, the control of hydrogen temperature is inhaled in room temperature, to reduce reacting for hydrogen and magnetic phase, pressure is 0-1MPa, then time 10-30 minute will be coated in magnet surface after heavy rare-earth oxide powder and alcohol mixing and ball milling, place into sintering in vacuum sintering furnace.The invention has the advantages that the magnet of Nd-Fe-B is absorbed protium at room temperature, the Nd-Fe-B magnet on surface layer is set to contain a certain amount of protium, then Dy or Tb oxide is sprayed on to the surface of Nd-Fe-B based sintered magnet, tempering reacts Dy or Tb oxide with the hydrogen in Grain-Boundary Phase first, it is significantly promoted so that magnet coercivity has, while increasing penetration depth.
Description
Technical field
The present invention relates to a kind of coercitive techniques of promotion Nd-Fe-B magnet.
Background technique
Sintered NdFeB magnet has high coercivity and magnetic energy product.Meanwhile sintered magnet microstructure and magnetic property
Uniformity consistency is good.So sintered NdFeB industrialized production ability is high.Chinese manufacturing enterprise has reached 170 according to statistics
More families, total production capacity have reached 3 hundreds of millions tons.It is widely used in new-energy automobile, railway transportation equipment, space flight and aviation dress
In the tradition such as standby, smart grid, energy-saving industrial motor and novel industry.But the Curie temperature of sintered NdFeB is low, temperature is steady
Qualitative difference constrains the application of neodymium iron boron.The coercivity for improving sintered magnet, the temperature stabilization for increasing magnet is developing new opplication
Important channel.
Improving the coercitive main method of sintered magnet is to add heavy rare earth Dy and Tb element, Dy/Tb substitution in neodymium iron boron
Nd element in magnet is formed (Nd, Dy/Tb)2Fe14B phase.The magnetocrystalline anisotropy field of the magnetism phase is greater than neodymium-iron-boron
Body can effectively improve magnet coercivity.But (Nd, Dy/Tb)2Fe14The remanent magnetism of B phase is low, and then influences the remanent magnetism of magnet
And maximum magnetic energy product.Therefore, reduce (Nd, Dy/Tb)2Fe14Ratio of the B phase in magnet, makes it be distributed in Nd2Fe14Outside B phase
Layer is formed (Nd, Dy/Tb)2Fe14B phase surrounds Nd2Fe14The core-shell structure of B, to increase the forming core field of magnet.The advantages of nucleocapsid
It is that coercivity increases the amplitude that obvious, remanent magnetism reduces and becomes smaller, reduces heavy rare earth usage amount.
Grain boundary decision is the method for realizing the structure.By the oxide containing heavy rare earth, fluoride, alloy, metal adsorption
On the moderate sintered magnet surface of thickness, after tempering, Dy/Tb enters the outer layer of crystal boundary and magnetic phase.
Method about grain boundary decision has " magnetron sputtering method ", " vapour deposition process ", " electrodeposition process ", " electrophoresis " and
" cladding process " " spray coating method " etc..Wherein, the equipment cost of magnetron sputtering and vapour deposition process is high, production efficiency is low.Electrodeposition process
It is by (Dy)2(OH)5NO3·nH2The compound depositions such as O are spread after heat resolve to the surface of magnet, the width that coercivity improves
It spends small.The raw material that electrophoresis uses is fluoride, is currently in laboratory stage.Cladding process and spray coating method are low for equipment requirements,
There are many factories to use the industrialization the method achieve grain boundary decision at present.The raw material one that cladding process and spray coating method use
As be fluoride or oxide.Hydride is also used in cladding process part.The preparation method of fluoride is the fluorination of oxide, together
Oxide is compared, and fluoride increases process procedure and pollution environment.Hydride be heavy rare earth element hydrogenation, be crushed preparation and
At, stability is poor, and it is inflammable in air, it needs to operate in the extremely low environment of oxygen content.So the use of oxide being directly work
The optimal selection that industry metaplasia produces.But the diffusion depth directly using the heavy rare earth of oxide is low.In order to improve diffusion depth, have
It reports CaH2It is spread with after the hybrid reaction of oxide, this CaH2With the reaction rate of oxide, expansion is largely affected
Depth is dissipated, is difficult to carry out industrialized production.
Summary of the invention
The purpose of the present invention is to provide a kind of coercitive techniques of promotion Nd-Fe-B magnet to be made using simple technique
With common reagent, grain boundary decision is carried out, the coercivity of magnet is improved.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions: a kind of promotion Nd-Fe-B magnetic
The coercitive technique of body, comprising the following steps:
A, after the magnet being sintered being needed to be cut into the shape of needs, pickling pretreatment is carried out；
B, it carries out inhaling hydrogen processing, the suction hydrogen process of magnet is carried out in the container with extraction gas for being connected with recirculated water,
The control of hydrogen temperature is inhaled in room temperature, to reduce reacting for hydrogen and magnetism phase, pressure 0-1MPa, time 10-30 minute；
C, the powder of heavy rare-earth oxide is mixed with alcohol, then carries out ball milling, ball milling granularity is 50nm-300nm；
D, the heavy rare-earth oxide powder that step C is obtained is applied to the magnet surface of step B in air, waits nature dry
It is dry；
E, the dusting magnet that step D is obtained is put into vacuum sintering furnace, reaches 10 to vacuum degree-3When Mpa, start to add
Heat carries out ageing treatment, and the temperature of level-one timeliness is 850 DEG C -1000 DEG C, and aging time is 8-10 hours, secondary aging temperature
It is 450 DEG C -550 DEG C, aging time is 3-5 hours, obtains finished product.
Preferably, magnet is placed in the container with extraction gas in the step B, reaches 10 to vacuum degree-3When Mpa,
Vacuum pump is closed, argon gas is passed through and starts gas washing, be passed through hydrogen after gas washing, when hydrogen pressure is 0.5Mpa, valve is closed, leads to
Recirculated water is crossed, cooling tube wall extracts extra hydrogen out, open valve after argon gas gas washing, magnet is taken after reacting 30 minutes
Out.Enable surface layer magnet containing the protium of appropriate amount, magnet is in the state of reducing agent when ensuring diffusion.
Preferably, in the step C, the powder of heavy rare-earth oxide is mixed with alcohol 1:1 in mass ratio.
Preferably, 300 revs/min of ball mill rotation revolving speed, Ball-milling Time 36 hours, ball milling granularity 100nm.
Preferably, level-one aging temp is 950 DEG C in the step E, and aging time is 10 hours；Secondary aging temperature is
450 DEG C, aging time is 3 hours.
Preferably, the heavy rare-earth oxide is Dy or Tb oxide.
Compared with prior art, the invention has the advantages that the magnet of Nd-Fe-B is absorbed protium at room temperature, make table
The Nd-Fe-B magnet of layer contains a certain amount of protium, Dy or Tb oxide is then sprayed on Nd-Fe-B based sintered magnet
Surface, tempering are reacted Dy or Tb oxide with the hydrogen in Grain-Boundary Phase first, are significantly promoted so that magnet coercivity has, simultaneously
Increase penetration depth.
Specific embodiment
The embodiment of the present invention is described below in detail, it is intended to be used to explain the present invention, and should not be understood as to of the invention
Limitation.
A kind of embodiment promoting the coercitive technique of Nd-Fe-B magnet, comprising the following steps:
A, after the magnet being sintered being needed to be cut into the shape of needs, pickling pretreatment is carried out；
B, it carries out inhaling hydrogen processing, magnet is placed in the container with extraction gas, reaches 10 to vacuum degree-3When Mpa, close
Vacuum pump is passed through argon gas and starts gas washing, is passed through hydrogen after gas washing, when hydrogen pressure is 0.5Mpa, valve is closed, by following
Ring water, cooling tube wall extract extra hydrogen out, open valve after argon gas gas washing, magnet is taken out after reacting 30 minutes；
C, the powder of Dy or Tb oxide is mixed with alcohol 1:1 in mass ratio, then carries out ball milling, ball mill is walked around certainly
300 revs/min of speed, Ball-milling Time 36 hours, ball milling granularity 100nm；
D, the heavy rare-earth oxide powder that step C is obtained is applied to the magnet surface of step B in air, is waited 20 minutes
Left and right spontaneously dries；
E, the dusting magnet that step D is obtained is put into vacuum sintering furnace, reaches 10 to vacuum degree-3When Mpa, start to add
Heat carries out ageing treatment, and level-one aging temp is 950 DEG C, and aging time is 10 hours；Secondary aging temperature is 450 DEG C, timeliness
Time is 3 hours, obtains finished product.
The result obtained with common manufacturing process in contrast, manufacturing process are as follows: by heavy rare-earth oxide and alcohol
It mixes, is placed in the tank of ball mill for 1:1 in mass ratio.Rotation revolving speed is 300 revs/min, ball milling 36 hours, is put down after ball milling
Equal granularity is 100nm.
The suspension of heavy rare earth is coated in the surface of magnet, it is 20 minutes dry.
Dried magnet is placed in vacuum sintering furnace, when vacuum degree reaches 10-3Mpa.It begins to warm up, when level-one
Imitating temperature is 950 DEG C, and aging time is 10 hours.Secondary aging temperature is 450 DEG C, and aging time is 3 hours.
| Remanent magnetism (kGs) | Coercivity (kOe) | Coercivity rises in value (kOe) | Magnetic energy product (MGOe) | |
| Example | 13.3 | 20.4 | 7.1 | 48.5 |
| Comparison | 13.2 | 17.2 | 4.0 | 47.6 |
Table 1
It is compared by table, after using technique of the invention, indices are obviously improved, by the magnetic of Nd-Fe-B
Body absorbs protium at room temperature, and the Nd-Fe-B magnet on surface layer is made to contain a certain amount of protium, then by Dy or Tb oxide
It is sprayed on the surface of Nd-Fe-B based sintered magnet, tempering reacts Dy or Tb oxide with the hydrogen in Grain-Boundary Phase first, so that magnetic
Body coercivity, which has, significantly to be promoted, while increasing penetration depth.
Above is only a specific embodiment of the present invention, but technical characteristic of the invention is not limited thereto, Ren Heben
Within the field of the present invention, made changes or modifications all cover within the scope of the patent of the present invention the technical staff in field.
Claims (6)
1. a kind of coercitive technique of promotion Nd-Fe-B magnet, it is characterised in that: the following steps are included:
A, after the magnet being sintered being needed to be cut into the shape of needs, pickling pretreatment is carried out；
B, it carries out inhaling hydrogen processing, the suction hydrogen process of magnet is carried out in the container with extraction gas for being connected with recirculated water, inhales hydrogen
Temperature control is in room temperature, to reduce reacting for hydrogen and magnetism phase, pressure 0-1MPa, time 10-30 minute；
C, the powder of heavy rare-earth oxide is mixed with alcohol, then carries out ball milling, ball milling granularity is 50nm-300nm；
D, the heavy rare-earth oxide powder that step C is obtained is applied to the magnet surface of step B in air, waits and spontaneously drying；
E, the dusting magnet that step D is obtained is put into vacuum sintering furnace, reaches 10 to vacuum degree-3When Mpa, begin to warm up, into
Row ageing treatment, the temperature of level-one timeliness are 850 DEG C -1000 DEG C, and aging time is 8-10 hours, secondary aging temperature 450
DEG C -550 DEG C, aging time is 3-5 hours, obtains finished product.
2. a kind of coercitive technique of promotion Nd-Fe-B magnet as described in claim 1, it is characterised in that: in the step B
Magnet is placed in the container with extraction gas, reaches 10 to vacuum degree-3When Mpa, vacuum pump is closed, argon gas is passed through and starts to wash
Gas is passed through hydrogen after gas washing, when hydrogen pressure is 0.5Mpa, closes valve, and by recirculated water, cooling tube wall works as reaction
After 30 minutes, extracts extra hydrogen out, open valve after argon gas gas washing, magnet is taken out.
3. a kind of coercitive technique of promotion Nd-Fe-B magnet as described in claim 1, it is characterised in that: the step C
In, the powder of heavy rare-earth oxide is mixed with alcohol 1:1 in mass ratio.
4. a kind of coercitive technique of promotion Nd-Fe-B magnet as claimed in claim 3, it is characterised in that: ball mill rotation
300 revs/min of revolving speed, Ball-milling Time 36 hours, ball milling granularity 100nm.
5. a kind of coercitive technique of promotion Nd-Fe-B magnet as described in claim 1, it is characterised in that: in the step E
Level-one aging temp is 950 DEG C, and aging time is 10 hours；Secondary aging temperature is 450 DEG C, and aging time is 3 hours.
6. a kind of coercitive technique of promotion Nd-Fe-B magnet as described in claim 1, it is characterised in that: the heavy rare earth
Oxide is Dy or Tb oxide.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111210987A (en) * | 2020-02-01 | 2020-05-29 | 厦门钨业股份有限公司 | R-T-B magnet material and preparation method and application thereof |
| CN111223623A (en) * | 2020-01-31 | 2020-06-02 | 厦门钨业股份有限公司 | Large-thickness neodymium iron boron magnetic steel and preparation method thereof |
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| CN1701396A (en) * | 2003-01-16 | 2005-11-23 | 爱知制钢株式会社 | Process for producing anisotropic magnet powder |
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| CN111223623A (en) * | 2020-01-31 | 2020-06-02 | 厦门钨业股份有限公司 | Large-thickness neodymium iron boron magnetic steel and preparation method thereof |
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Application publication date: 20191112 |