CN108417333A - A kind of IVU Nd-Fe-B permanent magnets and preparation method thereof - Google Patents
A kind of IVU Nd-Fe-B permanent magnets and preparation method thereof Download PDFInfo
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- CN108417333A CN108417333A CN201810134634.4A CN201810134634A CN108417333A CN 108417333 A CN108417333 A CN 108417333A CN 201810134634 A CN201810134634 A CN 201810134634A CN 108417333 A CN108417333 A CN 108417333A
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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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- 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
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- 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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- 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
- H01F41/0266—Moulding; Pressing
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Abstract
The present invention provides a kind of IVU Nd-Fe-B permanent magnets, by mass percent with Nd24.5‑aTb6.0‑bDybFe66.28+a+c‑gCo1.5‑ cNb0.2‑dZrdAl0.3‑e‑fGa0.1+eCu0.12+fB1.0+gThe composition of alloy of expression, wherein a=0~0.2；B=0~0.5；C=0~0.2；D=0~0.2；E=0~0.05；F=0~0.05；G=0~0.05.The present invention also provides the preparation methods of the IVU Nd-Fe-B permanent magnets, including carry out dispensing and obtained alloy powder according to by above-mentioned composition of alloy；By alloy powder compression moulding permanent magnet green compact are made；Permanent magnet green sintering is tempered so that the ripe base of permanent magnet is made；The ripe base of permanent magnet is machined so that Nd-Fe-B permanent magnet is made.The present invention Nd-Fe-B permanent magnet IVU available higher magnetic field peak value, more resistant to high temperature, can get preferable magnetic field consistency and develop operating cost it is low, have good cost performance.
Description
Technical field
The present invention relates to a kind of permanent magnet vacuum undulator (IVU) more particularly to a kind of IVU permanent magnets and preparation method thereof.
Background technology
Permanent magnet vacuum undulator (IVU) is the key equipment of third generation synchrotron radiation light source and free-electron laser device.
Since U.S. professor Halbach proposes permanent magnetism undulator new concept magnetic structure, nearly more than 30 years, it is based on various performance permanent magnetism waves
Swing the overwhelming majority that device occupies synchrotron radiation and free-electron laser undulator.In numerous permanent magnetism undulators, vacuum undulator
Large percentage, as permanent magnet vacuum undulator quantity nearly reaches 70% or more in synchrotron radiation light source；In free-electron laser
Field vacuum undulator quantity is also very much, and presents increase trend year by year over time.Large number of various permanent magnet vacuums
Undulator on-line operation provides sound assurance for the various rich and varied scientific experiments of synchrotron radiation user.
It is one of synchrotron radiation light source and free-electron laser vacuum undulator the main direction of development to pursue highfield.With
The progress of social technology, user also proposed synchrotron radiation light source and free-electron laser device vacuum undulator higher and higher
Requirement.The technical characterstic of the permanent magnet vacuum undulator of on-line operation is as shown in table 1 below both at home and abroad at present, includes mainly following several
Type：
● SmCo vacuum undulator
Its advantage is that undulator stable magnetic field, can higher temperature resistant baking, but peak magnetic field is relatively low that (operating point Mr exists
Between 1.05-1.10T), simultaneously because the birth defect of samarium cobalt permanent magnet body magnetic structure is to vacuum undulator magnetic field homogeneity such as phase
Position error, magnetic field integral etc. bring certain detrimental effect, constrain some scientific experiment demands of user.Exist both at home and abroad at present
The IVU majorities of line operation are SmCo vacuum undulators.
● neodymium iron boron vacuum undulator
Its advantage is that peak magnetic field has largely raising (generally about 5-25%), undulator magnetic field homogeneity compared to SmCo
Also it makes moderate progress, the disadvantage is that neodymium iron boron is subjected to easy ting produce after long-time high-temperature baking significantly demagnetizing.Neodymium iron boron is nearly tens
The new permanent-magnet that year occurs, is known as " magnetic king ", the stage that the technology of being currently under is constantly progressive.The neodymium iron boron of vacuum undulator
Comprehensive magnetic energy as can significantly promoted, be expected to substitution part CPMU.
1 various IVU of table (containing CPMU) canonical parameter
● neodymium (praseodymium) iron boron low temperature permanent magnetism undulator (CPMU)
CPMU generally uses neodymium iron boron or praseodymium iron boron permanent magnet as magnetic field sources at present.Its advantage is that cold operation magnetic field peak
Value can get and increase substantially (generally about 8-30%), and permanent magnet radiation resistance is excellent.But this several years research experiences show
CPMU also have magnetic field homogeneity bad (ordinary circumstance magnetic phase error be not so good as routine IVU), failure relatively frequently, develop run at
The shortcomings of this is high.The cryogenic system structure of special designing is also to the straight line of synchrotron radiation light source or free-electron laser device preciousness
Section brings certain length to lose；It needs to develop complicated low temperature geomagnetic survey system and low-temperature cooling system, it is expensive；And CPMU
To obtain highfield, general neodymium (praseodymium) iron boron permanent magnet not high using room temperature Hcj/Hk does not adapt to high temperature and toasts for a long time,
Poor hygienic in CPMU vacuum tanks, long-term accelerator on-line operation survival gas constantly " leakage ", influence vacuum degree improvement.Together
When IVU magnetic pole heads saturation effect, make CPMU deep cooling low temperature magnetic field increasing degree and permanent magnetism body hypothermia Br increasing degrees not at
Direct ratio causes Br larger " waste ".Have several CPMU on-line operations both at home and abroad at present.
The performance for improving permanent magnet vacuum undulator at present, there is following three kinds of research directions：
First, development and design comprehensive magnetic can be higher and the samarium cobalt permanent magnet body that has good stability, but combines domestic granddad
The data opened and consider from magnetic theory.This direction only exists theoretically possibility at present, and reality there's almost no operable
Property.
Second, using neodymium (praseodymium) iron boron low temperature negative temperature coefficient feature, development and design low temperature permanent magnetism undulator continues simultaneously
Improve permanent magnet comprehensive magnetic energy.It being illustrated before its technical characterstic, this respect is being continually striving to always both at home and abroad,
Achieve many achievements.
Third, the higher Nd-Fe-B permanent magnet of development and design comprehensive magnetic energy, this respect are also as described above, only Japanese
Equal a handful of countries have carried out this large amount of research, and are being continuously improved.From theoretical principle and technology operability,
The direction is also to be worth further furtheing investigate.
In the case of selecting the third higher permanent magnet of research direction development and design magnetic property, have in the world at present
A small amount of neodymium iron boron vacuum undulator on-line operation, but existing neodymium iron boron vacuum undulator is as shown in table 2 below, more or less exists
Certain technological deficiency：
Table 2 is both at home and abroad similar to the magnetic property technical indicator of IVU Nd-Fe-B permanent magnets
(1) Hcj of German IVU neodymium iron borons is very high, reaches 2700kA/m, but Br is relatively low that (operating point Mr only has 1.14T
Left and right) it is increased that IVU peak magnetic fields are compared with SmCo is not especially more.
(2) Br of Japan's IVU neodymium iron borons is relatively up to 1.25T or more (operating point Mr reaches 1.20T or so), but Hcj
Especially Hk is relatively low, and reserved IVU high-temperature bakings " safe temperature surplus " are not especially big, and temperature is toasted when being debugged to IVU
Degree control etc. brings certain difficulty.
(3) although the novel GBD neodymium iron borons Br that Some European synchrotron radiation light source IVU is used reaches 1.25T or more even
Higher, but GBD methods are only effective the case where Nd-Fe-B permanent magnet is orientated thinner thickness, and it is not suitable with all thickness neodymium iron borons
Permanent magnet, this makes application range be restricted, and main magnetic parameter (Br, Hcj, Hk etc.) etc. is also and without advantage.
Invention content
It is an object of the present invention to provide a kind of preparation method of IVU Nd-Fe-B permanent magnets, make to make using the Nd-Fe-B permanent magnet
There is higher magnetic field peak value for the IVU of magnetic field sources, more resistant to high temperature, magnetic field consistency is high, and it is cost-effective to develop operation.
The present invention is based on following directions to develop IVU Nd-Fe-B permanent magnets：There is high intrinsic coercivity Hcj/ developing
While the Nd-Fe-B permanent magnet of Hk and higher remanent magnetism Br, suitable control temperature coefficient (the mainly temperature coefficient of Hcj), in this way
Significantly decline even if Hcj/Hk has when high-temperature baking, but the surplus of trouble free service point and Hcj/Hk values be still it is enough, together
When can also reserve larger IVU high-temperature bakings " threshold temperature range ", to realize heat safe effect, comply with more extensive
High-end applications need.
The present invention provides a kind of IVU Nd-Fe-B permanent magnets, which is characterized in that it is by mass percent with Nd24.5- aTb6.0-bDybFe66.28+a+c-gCo1.5-cNb0.2-dZrdAl0.3-e-fGa0.1+eCu0.12+fB1.0+gThe composition of alloy of expression, wherein a=
0~0.2；B=0~0.5；C=0~0.2；D=0~0.2；E=0~0.05；F=0~0.05；G=0~0.05.
The Nd-Fe-B permanent magnet is Nd24.5Tb6.0Co1.5Fe66.28Nb0.2Al0.3Ga0.1Cu0.12B1.0, or
Nd24.5Tb6.0Co1.5Fe66.28Nb0.12Zr0.08Al0.3Ga0.1Cu0.12B1.0。
The surface of Nd-Fe-B permanent magnet is coated with TiN coating, which is 4-7 μm.
Further, the present invention also provides a kind of preparation method of IVU Nd-Fe-B permanent magnets, this method includes：
(1) according to by mass percent with
Nd24.5-aTb6.0-bDybFe66.28+a+c-gCo1.5-cNb0.2-dZrdAl0.3-e-fGa0.1+eCu0.12+fB1.0+gThe alloy of expression
Composition carries out dispensing and alloy powder is made, wherein a=0~0.2；B=0~0.5；C=0~0.2；D=0~0.2；E=0
~0.05；F=0~0.05；G=0~0.05；
(2) by alloy powder compression moulding permanent magnet green compact are made；
(3) permanent magnet green sintering is tempered so that the ripe base of permanent magnet is made；
(4) the ripe base of permanent magnet is machined so that Nd-Fe-B permanent magnet is made.
The step (1) is included in after dispensing is made rapid-hardening flake by rapid hardening belt-rejecting technology, then by the way that hydrogen is quick-fried and air-flow
Alloy powder is made in grinding process.
The step (2) includes carrying out orientation pressure using the pressure direction laterally vertical pressing mode vertical with magnetic direction
Type is made.
The step (3) is included in 1050-1070 DEG C of sintering, is tempered at 460-520 DEG C；Or be sintered at 1050-1060 DEG C,
Level-one tempering is carried out at 880-900 DEG C, and second annealing is carried out at 460-520 DEG C.
The step (4) includes uniformly removing the peel to carry out cutting processing by six faces, and machined surface is vertical with magnetic direction
Or it is parallel.
The preparation method of the IVU Nd-Fe-B permanent magnets further comprises step (5)：Using TiN coating to neodymium iron boron
Permanent magnet is sealed.
The preparation method of the IVU Nd-Fe-B permanent magnets further comprises step (6)：It is old using 145-155 DEG C of high temperature
Change mode carries out stabilization processes to Nd-Fe-B permanent magnet.
In the step (6), the processing time of high temperature ageing is 2-24 hours.
Step (1)-(3) carry out under low-oxygen environment.
The IVU Nd-Fe-B permanent magnets of the present invention have the beneficial effect that：
1) the Nd-Fe-B permanent magnet IVU based on the present invention can get higher magnetic field peak value.Conventional vacuum undulator SmCo
For room temperature operating point Mr between 1.05-1.10T, Nd-Fe-B permanent magnet room temperature operating point Mr of the invention reaches 1.22T or more.Phase
It is that increasing substantially for vacuum undulator peak magnetic field provides space to high Mr.And because of factors such as no magnetic pole head saturation effects,
It is " true " that neodymium iron boron Mr, which increases to the raising contribution of vacuum undulator (IVU) peak magnetic field,.
2) IVU Nd-Fe-B permanent magnets are more resistant to high temperature.The present invention IVU Nd-Fe-B permanent magnet room temperature Hk up to 2300kA/m with
On, in the case where Hk changes less even higher, the temperature coefficient of suitable control Hcj is in reduced levels, in addition, in conjunction with this hair
The cermet TiN coating that bright IVU Nd-Fe-B permanent magnets have makes the permanent magnet of the present invention more resistant to high temperature, to make use
The IVU of Nd-Fe-B permanent magnet manufacture of the present invention obtains ultra-high vacuum environment.
3) IVU Nd-Fe-B permanent magnets can get preferable magnetic field consistency.It is of the invention compared to existing samarium cobalt permanent magnet body
IVU Nd-Fe-B permanent magnet high-temperature bakings demagnetization synchronism is obviously improved.The magnetic fields IVU are padded in being greatly lowered for demagnetization amplitude
The improvement of magnetic phase error and field of integration is highly beneficial after benefit.
4) it is low to develop operating cost by the preparation of the Nd-Fe-B permanent magnet and IVU based on the permanent magnet, have good property
Valence ratio.The Nd-Fe-B permanent magnet of the present invention does not use the higher grain boundary decision method of cost, permanent magnet to prepare overall cost itself
The neodymium iron boron prepared better than general grain boundary decision.Further, since the Nd-Fe-B permanent magnet of the present invention can be used for more resistant to high-temperature baking
High performance IVU is made to replace the CPMU with similar performance.Relative to CPMU, the Nd-Fe-B permanent magnetic system based on the present invention
The IVU made, development and design, magnetic-field measurement, on-line operation need not develop expensive cryogenic system and magnetic field measurement system, and
On-line operation management is relatively easy on accelerator, has good superiority of effectiveness.
Description of the drawings
Fig. 1 is that 10 IVU Nd-Fe-B permanent magnets of the invention and 10 pass through with dimensions high-performance samarium cobalt permanent magnet body
The operating point intensity of magnetization (Mr) mean variation tendency chart of baking in 100-200 DEG C/24 hours.
Fig. 2 is that 10 IVU Nd-Fe-B permanent magnets of the invention and 10 pass through with dimensions high-performance samarium cobalt permanent magnet body
The rate of change tendency chart of the operating point intensity of magnetization (Mr) irreversible demagnetization of baking in 100-200 DEG C/24 hours.
Fig. 3 is the permanent magnet exemplar that 10 IVU Nd-Fe-B permanent magnets of the invention pass through baking in 100-200 DEG C/24 hours
Between the synchronous consistency, that is, discreteness situation map of operating point (Mr) demagnetization.
Fig. 4 is that 10 IVU Nd-Fe-B permanent magnets of the invention and 10 pass through with dimensions high-performance samarium cobalt permanent magnet body
100 DEG C/24 hours and 120 DEG C/24 hours twice after high-temperature baking the operating point intensity of magnetization (Mr) steadiness figure.
Fig. 5 is that 10 IVU Nd-Fe-B permanent magnets of the invention and 10 distinguish with dimensions high-performance samarium cobalt permanent magnet body
By 100 DEG C/24 hours and 120 DEG C/irreversible demagnetization consistency situation map after high-temperature baking for 24 hours.
Specific implementation mode
The present invention provides a kind of IVU Nd-Fe-B permanent magnets and preparation method thereof, the preparation sides of the IVU Nd-Fe-B permanent magnets
Method includes the following steps：
(1) dispensing is carried out according to composition of alloy and alloy powder is made
Composition of alloy is designed by high Br and high Hci principles, and improves material Curie temperature as far as possible, it is specific as follows：
I. use single alloy approach to ensure the uniformity of magnetic phase structure；
Ii. according to each element content of permanent magnet to it is magnetic mutually with it is non magnetic it is equal accurately calculate, obtain remanent magnetism Br
Theoretical value is 1.26T；
Iii. according to typical case R shown in table 32Fe14B phases Inner reports magnetic characteristic, illustrates that Nd elements can improve material Curie temperature
Degree, therefore use pure Nd elements；
3 typical case R of table2Fe14B phases Inner reports magnetic characteristic
| Magnetic phase type | Js(kGs) | Ha(kOe) | Density (g/cm3) | Tc(℃) |
| Pr2Fe14B | 15.6 | 75 | 7.54 | 292 |
| Nd2Fe14B | 16.0 | 73 | 7.60 | 312 |
| Tb2Fe14B | 7.0 | 220 | 7.96 | 347 |
| Dy2Fe14B | 7.1 | 150 | 8.05 | 325 |
Iv. optimize element T b, Dy content so that Tb is with Dy mass percents by original 2.5-3.5%, 2.5-4.0%
It is optimized to 5.5-6.0%, 0-0.5%, with high Br while to ensure product with high Hcj；
V. appropriate Co elements are added in permanent magnet to significantly improve material Curie temperature；
Vi. the elements such as trace of Al, Nb, Cu, Ga are added in permanent magnet, while inhibiting magnet crystal grain to grow up, keep crystal boundary rich
Rare earth distributed mutually is more continuous, easily prepared high Hcj, low-temperature coefficient permanent-magnet material.
The calculated results show with
Nd24.5-aTb6.0-bDybFe66.28+a+c-gCo1.5-cNb0.2-dZrdAl0.3-e-fGa0.1+eCu0.12+fB1.0+gThe alloy of expression
Composition can improve Hcj, Br and material Curie temperature while cost is reduced, and effect is to make material compared with high temperature resistant, in height
Temperature is lower still to retain higher Hcj, Br.Wherein, a=0~0.2；B=0~0.5；C=0~0.2；D=0~0.2；E=0~
0.05；F=0~0.05；G=0~0.05.Within this range, two IVU Nd-Fe-B permanent magnets that the present invention specifically uses are implemented
Example ingredient be：
A、Nd24.5Tb6.0Co1.5Fe66.28Nb0.2Al0.3Ga0.1Cu0.12B1.0
B、Nd24.5Tb6.0Co1.5Fe66.28Nb0.12Zr0.08Al0.3Ga0.1Cu0.12B1.0
After carrying out dispensing according to above-mentioned composition of alloy, rapid hardening thin slice is made with rapid hardening belt-rejecting technology in raw material, ensures speed
Solidifying piece ingredient is accurate and microstructure is uniform, to improve magnetic field symmetry；Then coarse crushing is carried out by HD process, then through gas
Grinding process fine grinding is flowed, by the alloy powder size distribution of alloy powder particle in more regular normal distribution, alloy powder is average
Granularity (SMD) is 3.0-3.5 μm (3.2 μm), and size distribution is more concentrated, to improve the side of the Nd-Fe-B permanent magnet of the present invention
Shape degree；Apparent density of powder is controlled in 1.8-2.5g/cm3, to reduce alloy powder apparent density, improve alloy powder and load
Even property, to improve magnetic field homogeneity.And the zinc stearate lubricant that addition mass percent is 0.025% thereto, uniformly
Mixing for standby use.
(2) by alloy powder compression moulding permanent magnet green compact are made
Alloy powder is put into the hypoxemia moulding press of inert gas shielding, is taken under the magnetic field of alignment magnetic field >=2T
To compression moulding be density it is 3.5-4.0g/cm3Oriented moulding green compact.
Wherein pressure direction makes green compact strictly be in electromagnet good place center perpendicular to magnetic direction, it is ensured that magnetic field
Direction both sides density of line of magnetic force is equal, so that subsequent mechanical is processed, and realizes the higher degree of orientation.By magnetic simulation calculate and
Experiments have shown that in green compact pressing process, die cavity upper and lower port (i.e. pressing direction) magnetic line of force distribution disorders lead to magnet compacting side
It is larger to both ends and centre degree of orientation difference, cause magnet corner part and central orientation degree deviation larger, be also easy to produce compared with
Big magnetic declination.To this suitable ripe base size of oriented moulding of design (ranging from 50-75mm (mold direction) × 25-35mm (compacting
Direction) × 20-55mm (magnetic field orientating direction)), such as the ripe base size 51.5mm (mold direction) of preferred orientation of the present invention molding
× 36mm (pressing direction) × 40.5mm (magnetic field orientating direction) ensures magnet pressing direction both ends, magnet corner part in
The core field degree of orientation≤1%, to reduce magnetization drift angle.
Due to the low oxygen process using inert gas shielding, it can be ensured that the oxygen content in sintered NdFeB permanent magnet iron is relatively low,
This improves the comprehensive magnetic energy of permanent magnet.In addition, after green compact compression moulding, usually also need to carry out isostatic cool pressing processing,
It is 4.5-5.0g/cm to obtain density3Isostatic cool pressing green compact.
(3) permanent magnet green sintering is tempered so that the ripe base of permanent magnet is made
To control crystal grain in smaller size range to obtain higher intrinsic coercivity Hcj, the present invention uses low-temperature sintering
With tempering process.After compression moulding by green compact at 1020-1070 DEG C vacuum-sintering 4-5h, then through 460-520 DEG C progress two level
It is heat-treated 4-5h；Or be sintered at 1050-1060 DEG C, level-one tempering is carried out at 880-900 DEG C, and two are carried out at 460-520 DEG C
Grade tempering, is made the ripe base of permanent magnet.
It is orientated the green compact that compacting is formed and forms ripe base after oversintering is tempered, the magnetic field of permanent magnet when reducing oriented moulding
Orientation disorder region, to reduce magnetization drift angle.In addition, at 1020-1070 DEG C at 4-5h and 460-520 DEG C 4-5h low temperature
Sintering and tempering, prevent magnet abnormal grain growth, ensure uniform shrinkage in liquid sintering process, realize higher orientation
Degree.
(4) the ripe base of permanent magnet is machined so that Nd-Fe-B permanent magnet is made
The ripe base of permanent magnet is machined, six faces are uniformly removed the peel, and reduce magnetic field orientating zone of turbulence, to ensure permanent magnetism
Iron has good N/S pole fields symmetry, smaller magnetization drift angle, good microscopic uniformity.Reinforce in ripe base mechanical processing process
Reference plane controls, and ensures that machined surface and magnetic direction angle are 90 ° or 180 °, to reduce magnetization drift angle, it is symmetrical to improve magnetic field
Property, realize high uniformity.In addition, a ripe base of permanent magnet can be regular by number is posted by being machined on magnetic field orientating direction
1 or 3 or 5 or 7 finished permanent magnets are cut into, to realize higher magnetic field symmetry and smaller magnetization drift angle.
(5) TiN coating and aging are used
Cermet TiN coating (4-7 μm thick) is plated through 450-470 DEG C/3-5 hours to above-mentioned surface of Nd-Fe-B permanent magnet,
Saturated magnetization after size appearance is examined, it is then old by 145-155 DEG C/2-24 hours day high temperature under half open circuit and idle condition
Change processing (i.e. all permanent magnet elements stabilization processes when, their N or S extremely all in one direction placement).
Preferably, the preparation method of the IVU Nd-Fe-B permanent magnets uses hypoxemia concatenation technique, and step (1)-(3) are low
It is carried out under oxygen environment, it is stringent to control alloy powder storage, pressing under magnetic field, green compact transhipment and enter the oxygen content during stove, make most
Whole magnet oxygen content≤800ppm, the magnetic property inhomogeneities for preventing surface or selective oxidation from bringing.
In above-mentioned steps, the present invention is by reducing at powder particle mean size and apparent density of powder and two level heat
Science and engineering skill, to obtain compared with high-orientation.
In addition, the present invention designs suitable ripe base size to ensure magnet pressing direction both ends, magnet corner by (1) design
Position and the central magnetic field degree of orientation≤1%, (2) carry out high-temperature heat treatment to reduce magnetic field orientating to being orientated the green compact that compacting is formed
Zone of turbulence, (3) uniformly peeling is to reduce magnetic field orientating zone of turbulence to six face of ripe base, and (4) are to ripe base mechanical processing process
Middle reinforcement reference plane control ensures that processing base face and direction of easy axis angle are 90 ° or 180 ° so that IVU neodymium iron of the invention
Boron permanent magnet has small magnetization drift angle.
In addition, the present invention also makes alloy powder size distribution in more regular normal distribution, alloy powder granularity by (1)
(SMD) it is 3-3.5 μm (3.2 μm average), and size distribution more concentrates (2) to use hypoxemia concatenation technique, strictly controls alloy
Powder storage, pressing under magnetic field, green compact are transported and enter the oxygen content during stove, make final magnet oxygen content≤800ppm, prevent
The magnetic property inhomogeneities that surface or selective oxidation are brought；(3) make alignment magnetic field >=2T during oriented moulding, simultaneously to the greatest extent
Alloy powder apparent density may be reduced, alloy powder is improved and load uniformity；(4) low temperature sintering technology is used, magnet is prevented
Abnormal grain growth ensures uniform shrinkage in liquid sintering process；(5) mechanical six faces of ripe base are uniformly removed the peel, reduces magnetic field and takes
To zone of turbulence and surface magnetism energy consistency large area so that IVU Nd-Fe-B permanent magnets of the invention have preferable magnetic
Field symmetry and smaller magnetization drift angle.
(1)-(5), IVU Nd-Fe-B permanent magnets of the invention are realized compared with high-orientation, small magnetic through the above steps as a result,
Change drift angle and preferable magnetic field symmetry improves Spatial Magnetic Fields Produced by Permanent Magnets quality to reach the feature of high uniformity.
Measurement result
It is prepared for two kinds of IVU Nd-Fe-B permanent magnets by the method for the invention：
A、Nd24.5Tb6.0Co1.5Fe66.28Nb0.2Al0.3Ga0.1Cu0.12B1.0, the room temperature Br of this IVU Nd-Fe-B permanent magnets
It is respectively 2754kA/m, 2361kA/m for 1.254T, Hcj and Hk.
B、Nd24.5Tb6.0Co1.5Fe66.28Nb0.12Zr0.08Al0.3Ga0.1Cu0.12B1.0, this IVU Nd-Fe-B permanent magnets it is normal
Warm Br is that 1.257T, Hcj and Hk are respectively 2571kA/m, 2355kA/m.
Composition vacuum undulator permanent magnet array is installed using above-mentioned Nd-Fe-B permanent magnet element as magnetic field sources, soft iron is adopted
It is saturated cobalt iron vanadium element with height, and and (is produced by Hangzhou Permanent Magnet Group Co., Ltd with dimensions high-performance samarium cobalt permanent magnet body
And the Mr of the samarium cobalt permanent magnet body of the domestic 30H models provided reaches 1.05T, and Hk reaches 1800kA/m or more) carry out complex art
Comparison, measurement result are as Figure 1-Figure 5.
Fig. 1-Fig. 2 respectively illustrates 10 IVU Nd-Fe-B permanent magnets of the invention and 10 with dimensions high-performance samarium
Cobalt permanent magnet passes through the measurement result of 100-200 DEG C/24 hours high temperature Halbach magnetic circuits baking, and wherein figure 1 illustrate operating points
The intensity of magnetization (Mr) mean variation trend, Fig. 2 shows the rate of change of the operating point intensity of magnetization (Mr) irreversible demagnetization to become
Gesture.Fig. 1 shows the IVU Nd-Fe-B permanent magnets of the present invention after 140 DEG C of high-temperature bakings, average total magnetic moment Mr just have it is certain under
Drop, Fig. 2 show the IVU Nd-Fe-B permanent magnets of the present invention after 150 DEG C of high-temperature bakings, and operating point magnetization M r is irreversible to move back
The ratio of magnetic is just more than samarium cobalt permanent magnet body.
Fig. 3 shows that 10 IVU Nd-Fe-B permanent magnets of the invention pass through the permanent magnet of baking in 100-200 DEG C/24 hours
Synchronous consistency, that is, discrete the implementations of operating point (Mr) demagnetization between exemplar.It can be seen in figure 3 that 10 IVU of the invention
Nd-Fe-B permanent magnet operating point magnetization M r values demagnetization after high-temperature baking synchronizes consistency, that is, discreteness in different temperatures
Section differs greatly：20 DEG C/24 hours following temperature, discreteness are minimum；120-140 DEG C/24 hours temperature ranges, discreteness is slightly
Deteriorate a little, but still is not especially big；140-200 DEG C/24 hours temperature ranges, discreteness deteriorate drastically.This illustrates this
The Nd-Fe-B permanent magnet prepared is invented in the fields the IVU operating temperature upper limit generally no more than 140 DEG C.
Fig. 4 shows 10 IVU Nd-Fe-B permanent magnets of the invention and 10 with dimensions high-performance samarium cobalt permanent magnet body
The steadiness of the operating point intensity of magnetization behind 100 DEG C/24 hours and 120 DEG C/24 hours twice high-temperature baking, from figure
It can be seen that the difference numerical value of the Mr of IVU Nd-Fe-B permanent magnets of the invention is substantially in 10Gs or so, this difference after secondary high-temperature
Value is mainly that (measurement accuracy of Helmholtz coil measured for the operating point intensity of magnetization is as caused by measurement error
0.1%)；This figure illustrates that, by high-temperature baking, significantly irreversible demagnetization is concentrated mainly on first day the operating point intensity of magnetization
Start some special time period, in the case of maintaining the condition of high temperature after 1 day, the operating point intensity of magnetization is not obviously moved back generally
Magnetic.
Fig. 5 shows 10 IVU Nd-Fe-B permanent magnets of the invention and 10 with dimensions high-performance samarium cobalt permanent magnet body
Respectively by 100 DEG C/24 hours and 120 DEG C/consistent implementations of irreversible demagnetization after high-temperature baking for 24 hours.From the figure, it can be seen that
In the 120 DEG C of bakings of IVU operating temperatures, 10 IVU Nd-Fe-B permanent magnets of the invention averagely demagnetization rate is 0.19% or so, unanimously
Property good (0.07-0.50%)；10 are 0.84% or so with dimensions high-performance samarium cobalt permanent magnet body averagely demagnetization rate, unanimously
Property is general
(0.45-1.29%).This illustrates the ratio of IVU Nd-Fe-B permanent magnets operating point Mr irreversible demagnetizations prepared by the present invention
Rate consistency, that is, discreteness is substantially better than samarium cobalt permanent magnet body, and the amplitude of irreversible demagnetization is also much smaller than samarium cobalt permanent magnet body.
The above, only presently preferred embodiments of the present invention, are not limited to the scope of the present invention, and of the invention is above-mentioned
Embodiment can also make a variety of changes.It is simple made by i.e. every claims applied according to the present invention and description
Single, equivalent changes and modifications, fall within the claims of patent of the present invention.The not detailed description of the present invention is normal
Advise technology contents.
Claims (12)
1. a kind of IVU Nd-Fe-B permanent magnets, which is characterized in that it is by mass percent with Nd24.5-aTb6.0-bDybFe66.28+a+c- gCo1.5-cNb0.2-dZrdAl0.3-e-fGa0.1+eCu0.12+fB1.0+gThe composition of alloy of expression, wherein a=0~0.2；B=0~0.5；c
=0~0.2；D=0~0.2；E=0~0.05；F=0~0.05；G=0~0.05.
2. IVU Nd-Fe-B permanent magnets as described in claim 1, which is characterized in that the Nd-Fe-B permanent magnet is
Nd24.5Tb6.0Co1.5Fe66.28Nb0.2Al0.3Ga0.1Cu0.12B1.0, or
Nd24.5Tb6.0Co1.5Fe66.28Nb0.12Zr0.08Al0.3Ga0.1Cu0.12B1.0。
3. IVU Nd-Fe-B permanent magnets as described in claim 1, which is characterized in that surface of Nd-Fe-B permanent magnet is coated with TiN platings
Layer, the thickness of coating are 4-7 μm.
4. a kind of preparation method of IVU Nd-Fe-B permanent magnets, which is characterized in that this approach includes the following steps：
(1) according to by mass percent with Nd24.5-aTb6.0-bDybFe66.28+a+c-gCo1.5-cNb0.2-dZrdAl0.3-e-fGa0.1+ eCu0.12+fB1.0+gThe composition of alloy of expression carries out dispensing and alloy powder is made, wherein a=0~0.2；B=0~0.5；C=0
~0.2；D=0~0.2；E=0~0.05；F=0~0.05；G=0~0.05；
(2) by alloy powder compression moulding permanent magnet green compact are made；
(3) permanent magnet green sintering is tempered so that the ripe base of permanent magnet is made；
(4) the ripe base of permanent magnet is machined so that Nd-Fe-B permanent magnet is made.
5. the preparation method of IVU Nd-Fe-B permanent magnets as claimed in claim 4, which is characterized in that the step (1) is included in
Rapid-hardening flake is made by rapid hardening belt-rejecting technology after dispensing, alloy powder then is made with air-flow grinding process by the way that hydrogen is quick-fried.
6. the preparation method of IVU Nd-Fe-B permanent magnets as claimed in claim 5, which is characterized in that the step (2) includes adopting
The laterally vertical pressing mode vertical with magnetic direction with pressure direction carries out orientation compression moulding.
7. the preparation method of IVU Nd-Fe-B permanent magnets as described in claim 4 or 5, which is characterized in that step (3) packet
It includes and is sintered at 1050-1070 DEG C, is tempered at 460-520 DEG C；Or be sintered at 1050-1060 DEG C, level-one is carried out at 880-900 DEG C returns
Fire, and second annealing is carried out at 460-520 DEG C.
8. the preparation method of IVU Nd-Fe-B permanent magnets as described in claim 4 or 5, which is characterized in that step (4) packet
It includes uniformly to remove the peel by six faces and carries out cutting processing, and machined surface and magnetic direction are perpendicular or parallel.
9. the preparation method of IVU Nd-Fe-B permanent magnets as described in claim 4 or 5, which is characterized in that further comprise step
(5)：Nd-Fe-B permanent magnet is sealed using TiN coating.
10. the preparation method of IVU Nd-Fe-B permanent magnets as claimed in claim 9, which is characterized in that further comprise step
(6)：Stabilization processes are carried out to Nd-Fe-B permanent magnet using 145-155 DEG C of high temperature ageing mode.
11. the preparation method of IVU Nd-Fe-B permanent magnets as claimed in claim 10, which is characterized in that in the step (6),
The processing time of high temperature ageing is 2-24 hours.
12. the preparation method of IVU Nd-Fe-B permanent magnets as described in claim 1, which is characterized in that step (1)-(3)
It is carried out under low-oxygen environment.
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| CN101982855A (en) * | 2010-09-16 | 2011-03-02 | 中国科学院宁波材料技术与工程研究所 | Sintered Nd-Fe-B permanent-magnet material and preparation method thereof |
| CN103489620A (en) * | 2013-10-15 | 2014-01-01 | 中国科学院上海应用物理研究所 | Praseodymium-Ferrum-Boron permanent magnet and preparation method thereof |
| CN106067358A (en) * | 2016-05-20 | 2016-11-02 | 江苏普隆磁电有限公司 | A kind of magnetic powder particle and preparation method thereof |
| CN106847494A (en) * | 2017-01-13 | 2017-06-13 | 中国科学院上海应用物理研究所 | High-performance permanent magnet preparation and the vacuum undulator magnetic structure containing the permanent magnet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101982855A (en) * | 2010-09-16 | 2011-03-02 | 中国科学院宁波材料技术与工程研究所 | Sintered Nd-Fe-B permanent-magnet material and preparation method thereof |
| CN103489620A (en) * | 2013-10-15 | 2014-01-01 | 中国科学院上海应用物理研究所 | Praseodymium-Ferrum-Boron permanent magnet and preparation method thereof |
| CN106067358A (en) * | 2016-05-20 | 2016-11-02 | 江苏普隆磁电有限公司 | A kind of magnetic powder particle and preparation method thereof |
| CN106847494A (en) * | 2017-01-13 | 2017-06-13 | 中国科学院上海应用物理研究所 | High-performance permanent magnet preparation and the vacuum undulator magnetic structure containing the permanent magnet |
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