CN108010705A - A kind of preparation method of neodymium iron boron magnetic body - Google Patents
A kind of preparation method of neodymium iron boron magnetic body Download PDFInfo
- Publication number
- CN108010705A CN108010705A CN201711223146.2A CN201711223146A CN108010705A CN 108010705 A CN108010705 A CN 108010705A CN 201711223146 A CN201711223146 A CN 201711223146A CN 108010705 A CN108010705 A CN 108010705A
- Authority
- CN
- China
- Prior art keywords
- neodymium iron
- iron boron
- magnetic body
- boron magnetic
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 68
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000009792 diffusion process Methods 0.000 claims abstract description 47
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 34
- 239000000956 alloy Substances 0.000 claims abstract description 34
- 238000007731 hot pressing Methods 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 238000011282 treatment Methods 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 7
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 238000002525 ultrasonication Methods 0.000 claims description 9
- 238000007654 immersion Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 230000005389 magnetism Effects 0.000 abstract description 12
- 150000007522 mineralic acids Chemical class 0.000 abstract description 5
- -1 TM Cu Inorganic materials 0.000 abstract 1
- 238000010792 warming Methods 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 34
- 150000002910 rare earth metals Chemical class 0.000 description 16
- 238000000034 method Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 10
- 238000012545 processing Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005324 grain boundary diffusion Methods 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 238000002955 isolation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 230000007480 spreading Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
- PXAWCNYZAWMWIC-UHFFFAOYSA-N [Fe].[Nd] Chemical compound [Fe].[Nd] PXAWCNYZAWMWIC-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- 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)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The present invention provides a kind of preparation method of neodymium iron boron magnetic body, including the basic neodymium iron boron magnetic body that thickness is 8~12mm is dried after dilute inorganic acid solution is handled；Diffusion alloy piece is attached to the upper and lower surface of dried basic neodymium iron boron magnetic body, then it is placed in hot pressing furnace, to hot pressing stove evacuation, when under vacuum conditions be warming up to 700~800 DEG C, start to apply 20~30MPa of pressure, and 7~10h of pressurize, then pressure release are vacuumized to normal pressure, again, 850~950 DEG C are continuously heating to, keeps the temperature 1~2h；Sample after diffusion is first made annealing treatment after different temperature in a vacuum furnace；Wherein described diffusion alloy piece is R1‑R2TM, wherein R1For Pr or Nd, R2For any one in Dy or Tb, TM Cu, Al, Zn or Fe.The present invention can produce the gratifying neodymium iron boron magnetic body of magnet coercivity, remanent magnetism and thickness of sample.
Description
Technical field
The present invention relates to magnet preparing technical field, more particularly to a kind of preparation method of neodymium iron boron magnetic body.
Background technology
As important Metallic Functional Materials, sintered NdFeB magnet is in space flight navigation, information electronics, the energy, traffic, logical
The various fields such as news, health care have a wide range of applications.In many fields, such as electric automobile, hybrid vehicle and wind-force
Need sintered NdFeB magnet that there is the coercivity of higher in the fields such as power generation, to meet the requirement under certain temperature.
Heavy rare earth is added with alloying, is formed (NdDy) of high magnetocrystalline anisotropy2Fe14B hard magnetic phases, can significantly improve
The coercivity of magnet, reduces magnetic property decay caused by high temperature, but at the same time, Dy atoms can form anti-iron with Fe atoms and couple, and make
Into the decline of remanent magnetism, under the extreme environment of permanent magnet at high temperature, the magnetic field intensity of generation can also decline.
As an improvement, the fluoride coating grain boundary decision for the dysprosium that researcher develops and the saturated vapor of dysprosium steam both at home and abroad
Vapour infiltration technology becomes the research hotspot of Sintered NdFeB magnet performance improvement.Patent CN200810179949.7, which is described, to be burnt
Tie magnet surface arrangement alloy powder, powder is rare earth intermetallic compound, heat treatment temperature for 20 DEG C~(Ts-10) DEG C, Ts
For the sintering temperature of sintered magnet.Sintered magnet includes the least part equal to or less than 20mm.Patent
CN200810179949.7 describes a kind of annealing device, using heavy rare earth (Tb, Dy, Ho) hydride, 700 DEG C~1000
Heavy rare earth element RH is diffused into inside sintered magnet between DEG C.However, for Sintered NdFeB magnet, current crystal boundary
The diffusion depth of infiltration technology is limited, and heavy rare earth element can not be diffused into inside large-size magnet, the size requirement to sample
Strictly, it can only generally handle thin slice magnet (within 5mm).The diffusion thickness for how improving grain boundary decision magnet is studied at present
Emphasis.
The content of the invention
It is an object of the invention to overcome drawbacks described above, there is provided one kind can produce magnet coercivity, remanent magnetism and sample
The preparation method of the gratifying neodymium iron boron magnetic body of thickness.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
The present invention provides a kind of preparation method of neodymium iron boron magnetic body, comprises the following steps：
Step 1：Business neodymium iron boron magnetic body is processed into 8~12mm thickness along orientation force direction, obtains basic neodymium iron boron magnetic body, so
Basic neodymium iron boron magnetic body is immersed in the hydrochloric acid solution that volumetric concentration is 3~5% afterwards or the nitric acid that volumetric concentration is 3~5% is molten
Dry 20~120min in liquid after 5~20min in 120~140 DEG C of environment；
Step 2：Diffusion alloy piece is attached to the upper and lower surface of the basic neodymium iron boron magnetic body after step 1 is handled, Ran Houfang
In hot pressing furnace, to hot pressing stove evacuation, treat that vacuum reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches 700
At~800 DEG C, start to apply 20~30MPa of pressure, and 7~10h of pressurize, then pressure release is to normal pressure, and hot pressing furnace again
Vacuumize, treat that vacuum reaches 1 × 10-2Below Pa, is continuously heating to 850~950 DEG C, keeps the temperature 1~2h；
Step 3：Sample after step 2 is spread is made annealing treatment under the conditions of 500~600 DEG C in a vacuum furnace, then
Made annealing treatment under the conditions of 400~450 DEG C, obtain target product；
Wherein described diffusion alloy piece is low melting point diffusion alloy R1-R2- TM, wherein R1For Pr or Nd, R2For Dy or Tb,
TM is any one in Cu, Al, Zn or Fe.
The beneficial effects of the present invention are：1) the method for the present invention to base magnet by carrying out inorganic acid solution immersion treatment
Afterwards, diffusion alloy is diffused with base magnet in the state of (700~800 DEG C) pressurizations (20~30MPa) of low temperature, pressure
Presence add melting diffusion alloy diffusion kinetic energy be distributed in heavy rare earth element grain boundary diffusion in melting diffusion alloy
Grain-Boundary Phase is simultaneously distributed in Grain-Boundary Phase, then by being diffused the heavy rare earth element so that there are Grain-Boundary Phase under high temperature (850~950)
Rich heavy rare earth metal shell structurre is being formed on main phase grain top layer, is realizing that heavy rare earth element enters principal phase as substitute element
It is interior, and in the boundary of principal phase, one continuous, region of high rare-earth content of formation, so that the coercivity of neodymium iron boron product
Significantly lifted, and remanent magnetism has little to no effect；Meanwhile after crystal boundary is permeated by heavy rare earth, crystal boundary Nd-rich phase is more continuous, more
It is clear to add, more efficient to isolation exchange-coupling interaction；(2) for the relatively traditional grain boundary decision method of the method for the present invention,
Diffusion depth is deeper, and the size requirement to spreading magnet is no so harsh, and applicability is wider, i.e., can be prepared by this method
The gratifying neodymium iron boron magnetic body of magnet coercivity, remanent magnetism and thickness of sample.
Embodiment
In order to describe the technical content, the structural feature, the achieved object and the effect of this invention in detail, below in conjunction with embodiment
It is explained in detail.
The design of most critical of the present invention is：By carrying out inorganic acid solution leaching to base magnet (common commercially available neodymium iron boron)
Heavy rare earth element grain boundary diffusion is promoted to make to be distributed in Grain-Boundary Phase under high temperature by low temperature pressuring method again after bubble processing
Heavy rare earth element rich rare earth element shell is formed on main phase grain top layer to prepare magnet coercivity, remanent magnetism and thickness of sample
Gratifying neodymium iron boron magnetic body.
The present invention provides a kind of preparation method of neodymium iron boron magnetic body, comprises the following steps：
Step 1：Business neodymium iron boron magnetic body is processed into 8~12mm thickness along orientation force direction, obtains basic neodymium iron boron magnetic body, so
Basic neodymium iron boron magnetic body is immersed in the hydrochloric acid solution that volumetric concentration is 3~5% afterwards or the nitric acid that volumetric concentration is 3~5% is molten
Dry 20~120min in liquid after 5~20min in 120~140 DEG C of environment；
Step 2：Diffusion alloy piece is attached to the upper and lower surface of the basic neodymium iron boron magnetic body after step 1 is handled, Ran Houfang
In hot pressing furnace, to hot pressing stove evacuation, treat that vacuum reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches 700
At~800 DEG C, start to apply 20~30MPa of pressure, and 7~10h of pressurize, then pressure release is to normal pressure, and hot pressing furnace again
Vacuumize, treat that vacuum reaches 1 × 10-2Below Pa, is continuously heating to 850~950 DEG C, keeps the temperature 1~2h；
Step 3：Sample after step 2 is spread is made annealing treatment under the conditions of 500~600 DEG C in a vacuum furnace, then
Made annealing treatment under the conditions of 400~450 DEG C, obtain target product；
Wherein described diffusion alloy piece is low melting point diffusion alloy R1-R2- TM, wherein R1For Pr or Nd, R2For Dy or Tb,
TM is any one in Cu, Al, Zn or Fe.
The present invention operation principle be：Existing neodymium iron boron magnetic body is selected to be cut into magnet based on 8~12mm thickness first, profit
With the oxide layer and oil stain for not having influential dilute hydrochloric acid solution or dilute nitric acid solution to remove base magnet to magnet performance, meanwhile,
Magnet after acid soak is dried peomotes heavy rare earth element in later stage diffusion alloy and adheres in magnet surface, Ran Houyu
Unlike conventional grain boundary decision (negative pressure, high temperature), then in the state of (700~800 DEG C) pressurizations (20~30MPa) of low temperature
It is diffused, the presence of pressure adds the diffusion kinetic energy of melting diffusion alloy, makes heavy rare earth element in melting diffusion alloy
(Tb/Dy) grain boundary diffusion is distributed in Grain-Boundary Phase and is distributed in Grain-Boundary Phase, meanwhile, pressure to a certain extent crystal boundary perpendicular to pressure
The direction (C axis) of power is broadening, and studies and show, is that diffusant is difficult to for the A faces of C direction of principal axis are from crystalline orientation
The face of attachment, broadening along C axis compensate for this shortcoming, then be diffused under high temperature (850~950) to a certain extent
So that the heavy rare earth element there are Grain-Boundary Phase is forming rich heavy rare earth metal shell structurre on main phase grain top layer, recycle first high
The mode of warm (500~600 DEG C) low temperature (400~450 DEG C) afterwards makes annealing treatment, all linked with one another between each step so that heavy rare earth is first
Element mutually enters in principal phase as substituting, and in the boundary of principal phase, forms a continuous, region for high rare-earth content, so that
The coercivity of neodymium iron boron product is set significantly to be lifted, and remanent magnetism has little to no effect.Meanwhile after crystal boundary is permeated by heavy rare earth, it is brilliant
Boundary's Nd-rich phase is more continuous, becomes apparent from, more efficient to isolation exchange-coupling interaction.
As can be seen from the above description, the beneficial effects of the present invention are：(1) the method for the present invention to base magnet by carrying out nothing
After machine acid solution immersion treatment, by diffusion alloy and base magnet (700~800 DEG C) pressurizations (20~30MPa) of low temperature shape
It is diffused under state, the diffusion kinetic energy that the presence of pressure adds melting diffusion alloy makes heavy rare earth element in melting diffusion alloy
Grain boundary diffusion is distributed in Grain-Boundary Phase and is distributed in Grain-Boundary Phase, then by being diffused under high temperature (850~950) so as to exist brilliant
The heavy rare earth element of boundary's phase is forming rich heavy rare earth metal shell structurre on main phase grain top layer, realizes that heavy rare earth element is used as and replaces
Enter for element in principal phase, and in the boundary of principal phase, one continuous, region of high rare-earth content of formation, so that neodymium iron
The coercivity of boron product is significantly lifted, and remanent magnetism has little to no effect；Meanwhile after crystal boundary is permeated by heavy rare earth, crystal boundary richness is dilute
It is native mutually more continuous, become apparent from, it is more efficient to isolation exchange-coupling interaction；(2) the method for the present invention tradition relatively is brilliant
For boundary's method of diffusion, diffusion depth is deeper, and the size requirement to spreading magnet is no so harsh, and applicability is wider, i.e., logical
The gratifying neodymium iron boron magnetic body of magnet coercivity, remanent magnetism and thickness of sample can be prepared by crossing this method.
Further, the concrete operations of step 1 are：It is molten that neodymium iron boron magnetic body is immersed in the hydrochloric acid that volumetric concentration is 3~5%
In liquid or salpeter solution, then the neodymium iron boron thin slice being immersed in hydrochloric acid solution or salpeter solution is surpassed under vacuum
5~10min of sonicated, dry 20~120min in 120~140 DEG C of environment.
Seen from the above description, when inorganic acid solution handles neodymium iron boron thin slice, ultrasound is carried out under vacuum
Ripple processing shortens soaking time and keeps vacuum environment at the same time, avoids occurring oxide layer in surface treatment process again and influencing
The attachment of later stage heavy rare earth element.
Further, the power of ultrasonication is 700~800W in step 1, and temperature is 40~50 DEG C.
Further, the thickness of the diffusion alloy piece is 0.1~0.25mm.
Further, the time made annealing treatment in step 3 under the conditions of 500~600 DEG C is 1~5h, at 400~450 DEG C
Under the conditions of time for making annealing treatment be 1~3h.
Embodiment 1
A kind of preparation method of neodymium iron boron magnetic body, comprises the following steps：
Step 1：Business neodymium iron boron magnetic body is processed into 5mm*10mm*8mm (8mm is thickness), obtains basic neodymium iron boron magnetic body
(it is described basis neodymium iron boron magnetic body composition by mass percentage be：Pr：5.9%；Nd：23.4%；Dy：1%；B：0.98%；
Al：0.1%；Cu：0.1%；Zr：0.1% and Fe：68.42%；), basic neodymium iron boron magnetic body then is immersed in volumetric concentration is
Ultrasonication is carried out in 3% hydrochloric acid solution and then under vacuum to the neodymium iron boron thin slice being immersed in hydrochloric acid solution
(power of ultrasonication is 700W, and temperature is 50 DEG C) 10min, the dry 120min in 120 DEG C of environment；
Step 2：(it is Pr by strip casting prepared composition by the diffusion alloy piece that thickness is 0.1mm50Tb20Cu30, (number
Value represent atomic percent) diffusion alloy) be attached to step 1 processing after basic neodymium iron boron magnetic body upper and lower surface, then
It is placed in hot pressing furnace, to hot pressing stove evacuation, treats that vacuum reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches
At 700 DEG C, start to apply pressure 30MPa, and pressurize 7h, then pressure release is to normal pressure, and hot pressing stove evacuation again, treats true
Reciprocal of duty cycle reaches 1 × 10-2Below Pa, is continuously heating to 850 DEG C, keeps the temperature 2h；
Step 3：Sample after step 2 is spread carries out annealing 5h under the conditions of 500 DEG C in a vacuum furnace, then at
Annealing 3h is carried out under the conditions of 400 DEG C, obtains target product.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Embodiment 2
Step 1：Business neodymium iron boron magnetic body is processed into 5mm*10mm*12mm (12mm is thickness), obtains basic neodymium-iron-boron
Body (it is described basis neodymium iron boron magnetic body composition by mass percentage be：Pr：5.9%；Nd：23.4%；Dy：1%；B：0.98%；
Al：0.1%；Cu：0.1%；Zr：0.1% and Fe：68.42%；), basic neodymium iron boron magnetic body then is immersed in volumetric concentration is
Ultrasonication is carried out in 5% salpeter solution and then under vacuum to the neodymium iron boron thin slice being immersed in salpeter solution
(power of ultrasonication is 800W, and temperature is 40 DEG C) 5min, the dry 20min in 140 DEG C of environment；
Step 2：(it is Pr by strip casting prepared composition by the diffusion alloy piece that thickness is 0.25mm50Tb20Cu30, (number
Value represent atomic percent) diffusion alloy) be attached to step 1 processing after basic neodymium iron boron magnetic body upper and lower surface, then
It is placed in hot pressing furnace, to hot pressing stove evacuation, treats that vacuum reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches
At 800 DEG C, start to apply pressure 20MPa, and pressurize 10h, then pressure release is to normal pressure, and hot pressing stove evacuation again, treats
Vacuum reaches 1 × 10-2Below Pa, is continuously heating to 950 DEG C, keeps the temperature 1h；
Step 3：Sample after step 2 is spread carries out annealing 1h under the conditions of 600 DEG C in a vacuum furnace, then at
Annealing 1h is carried out under the conditions of 450 DEG C, obtains target product.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Embodiment 3
Step 1：Business neodymium iron boron magnetic body is processed into 5mm*10mm*10mm (10mm is thickness), obtains basic neodymium-iron-boron
Body (it is described basis neodymium iron boron magnetic body composition by mass percentage be：Pr：5.9%；Nd：23.4%；Dy：1%；B：0.98%；
Al：0.1%；Cu：0.1%；Zr：0.1% and Fe：68.42%；), basic neodymium iron boron magnetic body then is immersed in volumetric concentration is
Ultrasonication is carried out in 4% hydrochloric acid solution and then under vacuum to the neodymium iron boron thin slice being immersed in hydrochloric acid solution
(power of ultrasonication is 750W, and temperature is 45 DEG C) 7min, the dry 60min in 130 DEG C of environment；
Step 2：(it is Pr by strip casting prepared composition by the diffusion alloy piece that thickness is 0.15mm50Tb20Cu30, (number
Value represent atomic percent) diffusion alloy) be attached to step 1 processing after basic neodymium iron boron magnetic body upper and lower surface, then
It is placed in hot pressing furnace, to hot pressing stove evacuation, treats that vacuum reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches
At 750 DEG C, start to apply pressure 25MPa, and pressurize 8h, then pressure release is to normal pressure, and hot pressing stove evacuation again, treats true
Reciprocal of duty cycle reaches 1 × 10-2Below Pa, is continuously heating to 900 DEG C, keeps the temperature 1.5h；
Step 3：Sample after step 2 is spread carries out annealing 3h under the conditions of 550 DEG C in a vacuum furnace, then at
Annealing 2h is carried out under the conditions of 420 DEG C, obtains target product.
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Comparative example 1
Original product (base magnet)
Detection：The magnetic parameter of test product, the results are shown in Table 1.
Comparative example 2
, with embodiment 2, difference is soaked in the processing in step 1 using alcohol, and is surpassed under normal pressure for other
Sonicated 10min；Pressurized treatments are not carried out in step 2.
Comparative example 3
, with embodiment 2, difference is soaked in the processing in step 1 using alcohol, and is surpassed under normal pressure for other
Sonicated 10min；High temperature diffusion is not carried out after the operation low temperature pressurized treatments of step 2 i.e.：By the diffusion that thickness is 0.15mm
Alloy sheet (is Pr by strip casting prepared composition50Tb20Cu30, the diffusion alloy of (numerical value expression atomic percent)) it is attached to
The upper and lower surface of basic neodymium iron boron magnetic body after step 1 processing, is then placed in hot pressing furnace, to hot pressing stove evacuation, treats vacuum
Degree reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches 750 DEG C, starts to apply pressure 25MPa, and pressurize 8h.
The parameter of 1 1~embodiment of embodiment 3 of table and comparative example product.
As shown in Table 1, which transforms to thicker basic neodymium iron boron magnetic body, still can be bright
The aobvious intrinsic coercivity for improving neodymium iron boron magnetic body, and the influence to remanent magnetism is minimum, has little influence on.
In conclusion the preparation method of neodymium iron boron magnetic body provided by the invention, molten by carrying out inorganic acid to base magnet
After liquid immersion treatment, by diffusion alloy and base magnet in the state of (700~800 DEG C) pressurizations (20~30MPa) of low temperature into
Row diffusion, the diffusion kinetic energy that the presence of pressure adds melting diffusion alloy make in melting diffusion alloy heavy rare earth element along crystal boundary
Diffusion profile is in Grain-Boundary Phase and is distributed in Grain-Boundary Phase, then by being diffused under high temperature (850~950) so that there are Grain-Boundary Phase
Heavy rare earth element is forming rich heavy rare earth metal shell structurre on main phase grain top layer, realizes heavy rare earth element as substitute element
Into in principal phase, and in the boundary of principal phase, one continuous, region of high rare-earth content of formation, so that neodymium iron boron product
Coercivity significantly lifted, and remanent magnetism has little to no effect；Meanwhile after crystal boundary is permeated by heavy rare earth, crystal boundary Nd-rich phase is more
Add continuously, become apparent from, it is more efficient to isolation exchange-coupling interaction；The relatively traditional grain boundary decision method of the method for the present invention
For, diffusion depth is deeper, and the size requirement to spreading magnet is no so harsh, and applicability is wider, that is, passes through this method energy
Prepare the gratifying neodymium iron boron magnetic body of magnet coercivity, remanent magnetism and thickness of sample.
The foregoing is merely the embodiment of the present invention, is not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made, is directly or indirectly used in other relevant technology necks
Domain, is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of neodymium iron boron magnetic body, it is characterised in that comprise the following steps：
Step 1：Business neodymium iron boron magnetic body is processed into 8~12mm thickness along orientation force direction, basic neodymium iron boron magnetic body is obtained, then will
Basic neodymium iron boron magnetic body is immersed in 5 in the hydrochloric acid solution that volumetric concentration is 3~5% or the salpeter solution that volumetric concentration is 3~5%
20~120min is dried after~20min in 120~140 DEG C of environment；
Step 2：Diffusion alloy piece is attached to the upper and lower surface of the basic neodymium iron boron magnetic body after step 1 is handled, is then placed on heat
Press in stove, to hot pressing stove evacuation, treat that vacuum reaches 1 × 10-2Below Pa, heats up hot pressing furnace, when temperature reaches 700~
At 800 DEG C, start to apply 20~30MPa of pressure, and 7~10h of pressurize, then pressure release is to normal pressure, and hot pressing furnace is taken out again
Vacuum, treats that vacuum reaches 1 × 10-2Below Pa, is continuously heating to 850~950 DEG C, keeps the temperature 1~2h；
Step 3：Sample after step 2 is spread is made annealing treatment under the conditions of 500~600 DEG C in a vacuum furnace, then at 400
Made annealing treatment under the conditions of~450 DEG C, obtain target product；
Wherein described diffusion alloy piece is low melting point diffusion alloy R1-R2- TM, wherein R1For Pr or Nd, R2It is for Dy or Tb, TM
Any one in Cu, Al, Zn or Fe.
2. the preparation method of neodymium iron boron magnetic body according to claim 1, it is characterised in that the concrete operations of step 1 are：Will
Neodymium iron boron magnetic body is immersed in the hydrochloric acid solution or salpeter solution that volumetric concentration is 3~5%, then under vacuum to immersion
Neodymium iron boron thin slice in hydrochloric acid solution or salpeter solution carries out 5~10min of ultrasonication, in 120~140 DEG C of environment
Dry 20~120min.
3. the preparation method of neodymium iron boron magnetic body according to claim 2, it is characterised in that ultrasonication in step 1
Power is 700~800W, and temperature is 40~50 DEG C.
4. the preparation method of neodymium iron boron magnetic body according to claim 1, it is characterised in that the thickness of the diffusion alloy piece
For 0.1~0.25mm.
5. the preparation method of neodymium iron boron magnetic body according to claim 1, it is characterised in that at 500~600 DEG C in step 3
Under the conditions of time for making annealing treatment be 1~5h, the time made annealing treatment under the conditions of 400~450 DEG C is 1~3h.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711223146.2A CN108010705B (en) | 2017-11-29 | 2017-11-29 | Preparation method of neodymium iron boron magnet |
| CN202010631985.3A CN111710519B (en) | 2017-11-29 | 2017-11-29 | Method for preparing neodymium-iron-boron magnet through grain boundary diffusion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711223146.2A CN108010705B (en) | 2017-11-29 | 2017-11-29 | Preparation method of neodymium iron boron magnet |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010631985.3A Division CN111710519B (en) | 2017-11-29 | 2017-11-29 | Method for preparing neodymium-iron-boron magnet through grain boundary diffusion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108010705A true CN108010705A (en) | 2018-05-08 |
| CN108010705B CN108010705B (en) | 2020-08-04 |
Family
ID=62054453
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010631985.3A Active CN111710519B (en) | 2017-11-29 | 2017-11-29 | Method for preparing neodymium-iron-boron magnet through grain boundary diffusion |
| CN201711223146.2A Active CN108010705B (en) | 2017-11-29 | 2017-11-29 | Preparation method of neodymium iron boron magnet |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010631985.3A Active CN111710519B (en) | 2017-11-29 | 2017-11-29 | Method for preparing neodymium-iron-boron magnet through grain boundary diffusion |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN111710519B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110111961A (en) * | 2019-03-12 | 2019-08-09 | 宁波雄海稀土速凝技术有限公司 | A kind of the neodymium-iron-boron preparation and its neodymium iron boron magnetic body of high-coercive force |
| CN110136953A (en) * | 2019-06-17 | 2019-08-16 | 江苏科技大学 | A kind of preparation method with the compound neodymium iron boron magnetic body of coercivity gradient distribution |
| CN110556244A (en) * | 2019-08-27 | 2019-12-10 | 安徽省瀚海新材料股份有限公司 | Process for preparing high-coercivity neodymium-iron-boron magnet by diffusion method |
| CN111161950A (en) * | 2020-03-19 | 2020-05-15 | 浙江凯文磁业有限公司 | Pretreatment device and treatment process for grain boundary permeation of heavy rare earth |
| CN112941457A (en) * | 2021-01-21 | 2021-06-11 | 华南理工大学 | Alloy composite grain boundary diffusant for neodymium iron boron magnet and preparation method and application thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112420305A (en) * | 2020-11-10 | 2021-02-26 | 四川大学 | Grain boundary diffusion method for improving magnetic property of rare earth permanent magnetic material |
| CN113380528B (en) * | 2021-06-15 | 2022-08-19 | 中钢天源股份有限公司 | Method for remolding sintered neodymium iron boron grain boundary |
| CN113571279B (en) * | 2021-07-23 | 2024-05-03 | 包头天和磁材科技股份有限公司 | Magnet and method for manufacturing the same |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009087975A1 (en) * | 2008-01-11 | 2009-07-16 | Intermetallics Co., Ltd. | PROCESS FOR PRODUCTION OF NdFeB SINTERED MAGNETS AND NDFEB SINTERED MAGNETS |
| CN101542654A (en) * | 2007-03-30 | 2009-09-23 | Tdk株式会社 | Process for producing magnet |
| CN102181820A (en) * | 2011-06-16 | 2011-09-14 | 安徽大地熊新材料股份有限公司 | Method for enhancing coercivity of neodymium-iron-boron magnet material |
| CN104064346A (en) * | 2014-05-30 | 2014-09-24 | 宁波同创强磁材料有限公司 | NdFeB magnet and preparation method thereof |
| CN104388951A (en) * | 2014-11-24 | 2015-03-04 | 上海交通大学 | Grain boundary diffusion method for improving properties of sintered NdFeB magnets |
| CN106409497A (en) * | 2016-08-31 | 2017-02-15 | 浙江东阳东磁稀土有限公司 | Grain boundary diffusion method for neodymium-iron-boron magnet |
| CN107256795A (en) * | 2017-06-27 | 2017-10-17 | 北京科技大学 | The method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4433282B2 (en) * | 2004-01-23 | 2010-03-17 | Ｔｄｋ株式会社 | Rare earth magnet manufacturing method and manufacturing apparatus |
| CN104851545B (en) * | 2015-05-21 | 2017-11-17 | 王怡 | A kind of permanent-magnet material preparation method with grain boundary decision layer |
| CN105755441B (en) * | 2016-04-20 | 2019-01-11 | 中国科学院宁波材料技术与工程研究所 | A kind of method that magnetron sputtering method expands infiltration heavy rare earth raising coercivity of sintered ndfeb |
-
2017
- 2017-11-29 CN CN202010631985.3A patent/CN111710519B/en active Active
- 2017-11-29 CN CN201711223146.2A patent/CN108010705B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101542654A (en) * | 2007-03-30 | 2009-09-23 | Tdk株式会社 | Process for producing magnet |
| WO2009087975A1 (en) * | 2008-01-11 | 2009-07-16 | Intermetallics Co., Ltd. | PROCESS FOR PRODUCTION OF NdFeB SINTERED MAGNETS AND NDFEB SINTERED MAGNETS |
| CN102181820A (en) * | 2011-06-16 | 2011-09-14 | 安徽大地熊新材料股份有限公司 | Method for enhancing coercivity of neodymium-iron-boron magnet material |
| CN104064346A (en) * | 2014-05-30 | 2014-09-24 | 宁波同创强磁材料有限公司 | NdFeB magnet and preparation method thereof |
| CN104388951A (en) * | 2014-11-24 | 2015-03-04 | 上海交通大学 | Grain boundary diffusion method for improving properties of sintered NdFeB magnets |
| CN106409497A (en) * | 2016-08-31 | 2017-02-15 | 浙江东阳东磁稀土有限公司 | Grain boundary diffusion method for neodymium-iron-boron magnet |
| CN107256795A (en) * | 2017-06-27 | 2017-10-17 | 北京科技大学 | The method that performance Nd Fe B sintered magnet is prepared using two step grain boundary diffusion process |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110111961A (en) * | 2019-03-12 | 2019-08-09 | 宁波雄海稀土速凝技术有限公司 | A kind of the neodymium-iron-boron preparation and its neodymium iron boron magnetic body of high-coercive force |
| CN110111961B (en) * | 2019-03-12 | 2024-03-12 | 宁波雄海稀土速凝技术有限公司 | Preparation method of high-coercivity neodymium-iron-boron magnet and neodymium-iron-boron magnet |
| CN110136953A (en) * | 2019-06-17 | 2019-08-16 | 江苏科技大学 | A kind of preparation method with the compound neodymium iron boron magnetic body of coercivity gradient distribution |
| CN110136953B (en) * | 2019-06-17 | 2022-04-26 | 江苏科技大学 | Preparation method of composite neodymium iron boron magnet with coercivity gradient distribution characteristic |
| CN110556244A (en) * | 2019-08-27 | 2019-12-10 | 安徽省瀚海新材料股份有限公司 | Process for preparing high-coercivity neodymium-iron-boron magnet by diffusion method |
| CN111161950A (en) * | 2020-03-19 | 2020-05-15 | 浙江凯文磁业有限公司 | Pretreatment device and treatment process for grain boundary permeation of heavy rare earth |
| CN111161950B (en) * | 2020-03-19 | 2024-05-07 | 浙江凯文磁业有限公司 | Pretreatment device and treatment process for heavy rare earth grain boundary permeation |
| CN112941457A (en) * | 2021-01-21 | 2021-06-11 | 华南理工大学 | Alloy composite grain boundary diffusant for neodymium iron boron magnet and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111710519B (en) | 2022-09-20 |
| CN111710519A (en) | 2020-09-25 |
| CN108010705B (en) | 2020-08-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108010705A (en) | A kind of preparation method of neodymium iron boron magnetic body | |
| JP5870522B2 (en) | Method for manufacturing permanent magnet | |
| CN105185501B (en) | The manufacture method of rare earth permanent-magnetic material | |
| CN103456451B (en) | A kind of preparation method of the corrosion-resistant sintered NdFeB of room temperature high energy product | |
| CN102347126B (en) | High-performance sintered neodymium-iron-boron (Nd-Fe-B) rare-earth permanent magnet material and manufacturing method thereof | |
| CN104795228B (en) | A kind of method that grain boundary decision Dy Cu alloys prepare high-performance neodymium-iron-boron magnet | |
| CN105321702B (en) | One kind improves the coercitive method of sintered NdFeB magnet | |
| CN104388952B (en) | It is a kind of to accelerate Sintered NdFeB magnet surface Dy/Tb adhesion layers to expand the method oozed | |
| CN104388951A (en) | Grain boundary diffusion method for improving properties of sintered NdFeB magnets | |
| CN105655075B (en) | A kind of method that high temperature insostatic pressing (HIP) obtains high magnetic sintered NdFeB | |
| CN105869876B (en) | A kind of rare-earth permanent magnet and its manufacture method | |
| JP2013175705A (en) | Method of manufacturing rare earth magnet | |
| CN105742048B (en) | The method that a kind of ion implanting rare earth and alloy improve Sintered NdFeB magnet performance | |
| CN108899149A (en) | A kind of efficient diffusion of heavy rare earth Dy for high-coercive force neodymium iron boron magnetic body method | |
| CN107799294B (en) | A kind of method that grain boundary decision prepares neodymium iron boron magnetic body | |
| CN106128676B (en) | A kind of sintering method of neodymium iron boron magnetic body | |
| CN102568806A (en) | Method for preparing rare-earth permanent magnets by infiltration process and graphite box utilized in method | |
| KR20200060444A (en) | Rare earth permanent magnet material and manufacturing method thereof | |
| CN105957706A (en) | Method for preparing high-performance neodymium iron boron magnet by pressure impregnation of Dy<3+>/Tb<3+> | |
| CN103219146B (en) | Method for enhancing magnet performance through reducing-dispersing method | |
| KR20170013744A (en) | Method for manufacturing rare earth sintered magnet using low melting point elements | |
| CN101901658A (en) | Sintered NdFeB rare-earth permanent magnet material with modified grain boundary phase and preparation method thereof | |
| CN107564723A (en) | The preparation method of high-coercive force neodymium iron boron magnetic body | |
| CN104425092B (en) | A kind of neodymium-iron-boron magnetic material and preparation method thereof | |
| CN110364352A (en) | A kind of preparation method of Nd-Fe-B permanent magnet material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PP01 | Preservation of patent right | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20210623 Granted publication date: 20200804 |
|
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20211223 Granted publication date: 20200804 |
|
| PD01 | Discharge of preservation of patent | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20211223 Granted publication date: 20200804 |
|
| PP01 | Preservation of patent right | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20230223 Granted publication date: 20200804 |
|
| PD01 | Discharge of preservation of patent |