CN105761861B - A kind of neodymium iron boron magnetic body and preparation method thereof - Google Patents
A kind of neodymium iron boron magnetic body and preparation method thereof Download PDFInfo
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- CN105761861B CN105761861B CN201610305312.2A CN201610305312A CN105761861B CN 105761861 B CN105761861 B CN 105761861B CN 201610305312 A CN201610305312 A CN 201610305312A CN 105761861 B CN105761861 B CN 105761861B
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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
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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
- H01F1/0576—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 pressed, e.g. hot working
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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
- H01F41/026—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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- 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
- H01F41/0266—Moulding; Pressing
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Abstract
The present invention provides a kind of neodymium iron boron magnetic bodies, including neodymium iron boron magnetic body blank and the RTMH alloy-layer for being compounded in its surface；The R is selected from one of rare earth element or a variety of；The T is Fe and/or Co；The M is selected from one of Al, Si, Ti, V, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta, W, Pt, Au, Pb and Bi or a variety of；The H is protium.The present invention, which uses, coats RTMH alloy-layer on neodymium iron boron magnetic body surface, not only alloy firm layer is formed in magnet surface, and grain boundary decision infiltration can be generated at border, so that the coercivity of magnet is improved significantly, and it can guarantee that the original remanent magnetism of magnet and maximum magnetic energy product do not occur significantly to reduce.
Description
Technical field
The invention belongs to magnet preparation technical fields more particularly to a kind of neodymium iron boron magnetic body and preparation method thereof.
Background technique
Magnet is the substance that can generate magnetic field, has the characteristic for attracting the metals such as ferromagnetic material such as iron, nickel, cobalt.Magnetic
Body is generally divided into permanent magnet and soft magnetic bodies, and the material as magnetizer and electromagnet is mostly soft magnetic bodies, and polarity is with added
Polarity of the magnetic field and change；And permanent magnet, that is, hard magnetic body, its magnetic magnet can be kept for a long time, be not easy loss of excitation, be also not easy by
Magnetization.Thus, either industrial production still in daily life, one of most common muscle material of hard magnetic body.
Hard magnetic body can be divided into natural magnet and artificial magnet, and artificial magnet refers to can by the alloy for synthesizing different materials
With reach with natural magnet (magnet) identical effect, but also magnetic force can be improved.Early in 18th century, there have been artificial
Magnet, but the process for manufacturing more strong magnetic material is very slowly, produces alnico magnet until the 1930s
(AlNiCo), just make it possible the large-scale application of magnet.Then, the 1950s is manufactured that ferrite
(Ferrite), the sixties, the appearance of rare earth permanent magnet then open a new era, first generation samarium cobalt permanent magnet for the application of magnet
SmCo5, second generation precipitation hardenable samarium cobalt permanent magnet Sm2Co17, so far, develop to third generation Nd-Fe-B permanent magnet material
(NdFeB).Although current ferrimagnet is still the maximum permanent-magnet material of dosage, the output value of neodymium iron boron magnetic body is significantly super
Ferrite permanent-magnet materials are crossed, a big industry is had evolved into.
Neodymium iron boron magnetic body is also referred to as neodymium magnet (Neodymium magnet), chemical formula Nd2Fe14B is a kind of artificial
Permanent magnet, and so far with the permanent magnet of most strong magnetic force, maximum magnetic energy product (BHmax) exceeds ferrite 10
Times or more, in the state of naked magnetic, magnetic force can reach 3500 Gauss.The advantages of neodymium iron boron magnetic body is cost performance height, body
The advantages of the features such as small, light-weight, good mechanical property of product and strong magnetism, such high-energy density, makes Nd-Fe-B permanent magnet material
It is had been widely used in modern industry and electronic technology, is known as magnetic king in magnetics circle.Thus, neodymium iron boron magnetic body is answered
The focus always given more sustained attention in the industry with extension.
After decades of development, the magnetic property of Sintered NdFeB magnet is continuously improved, wherein remanent magnetism Br and maximum magnetic energy
(BH) max is already close to limiting value for product, however the practical coercivity of Sintered NdFeB only has 30% of theoretical value or so, therefore, mention
High-coercive force is the key that improve Sintered NdFeB magnet comprehensive performance.And coercitive method is improved at present and is mainly passed through directly
Heavy rare earth is added in melting to improve coercivity, but this method can be substantially reduced on the basis of improving coercitive remanent magnetism and
Magnetic energy product.
Therefore, a kind of more suitable method how is found to improve coercivity, but is able to maintain remanent magnetism and maximum magnetic energy
Product, is always the focus of research and development type neodymium iron boron magnetic body manufacturing enterprise extensive concern in the industry.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that provide a kind of neodymium iron boron magnetic body and preparation method thereof, this
The preparation method simple process provided is provided, can effectively improve the coercivity of neodymium iron boron magnetic body, additionally it is possible to keep magnet
Remanent magnetism and maximum magnetic energy product.
The present invention provides a kind of neodymium iron boron magnetic bodies, including neodymium iron boron magnetic body blank and the RTMH alloy for being compounded in its surface
Layer；
The R is selected from one of rare earth element or a variety of；
The T is Fe and/or Co；
The M be selected from Al, Si, Ti, V, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta,
W, one of Pt, Au, Pb and Bi or a variety of；
The H is protium.
Preferably, include: in the RTMH alloy-layer
50~100 parts by weight of R；
T is less than or equal to 44 parts by weight；
M is less than or equal to 49 parts by weight；
H is less than or equal to 2 parts by weight.
Preferably, the quality of the RTMH alloy-layer account for the neodymium iron boron magnetic body gross mass ratio be less than or equal to
5%.
Preferably, each ingredient forms by mass percentage in the neodymium iron boron magnetic body blank, comprising: and Pr-Nd:28%~
33%；Dy:0~10%；Tb:0~10%；Nb:0~5%；B:0.5%~2.0%；Al:0~3.0%；Cu:0~1%；Co:
0~3%；Ga:0~2%；Gd:0~2%；Ho:0~2%；Zr:0~2%；Surplus is Fe.
It preferably, further include one of other rare earth elements or a variety of in the ingredient of the neodymium iron boron magnetic body blank.
The present invention provides a kind of preparation methods of neodymium iron boron magnetic body, comprising the following steps:
A after) mixing RTMH alloy powder with organic solvent, suspension is obtained；
The R is selected from one of rare earth element or a variety of；The T is Fe and/or Co；The M be selected from Al, Si, Ti, V,
One of Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta, W, Pt, Au, Pb and Bi or a variety of；
The H is protium；
B) suspension for obtaining above-mentioned steps is coated in neodymium iron boron blank surface, obtains semi-finished product；
C after) semi-finished product for obtaining above-mentioned steps are heat-treated, neodymium iron boron magnetic body is obtained.
Preferably, the average particle size of the RTMH alloy powder is 1~20 μm；The organic solvent includes gasoline, ethyl alcohol
With one of acrylic acid or a variety of.
Preferably, the mixed temperature is 15~35 DEG C, and the mixed time is 7~17 hours.
Preferably, the heat treatment includes High temperature diffusion processing and lonneal processing.
Preferably, the temperature of the High temperature diffusion processing is 700~1000 DEG C, and the time of the High temperature diffusion processing is 3
~20 hours；
The temperature of the lonneal processing is 350~750 DEG C, and the time of the lonneal processing is 1~8 hour.
The present invention provides a kind of neodymium iron boron magnetic bodies, including neodymium iron boron magnetic body blank and the RTMH alloy for being compounded in its surface
Layer；The R is selected from one of rare earth element or a variety of；The T is Fe and/or Co；The M be selected from Al, Si, Ti, V, Cr,
One of Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta, W, Pt, Au, Pb and Bi or a variety of；Institute
Stating H is protium.Compared with prior art, the present invention, which uses, coats RTMH alloy-layer on neodymium iron boron magnetic body surface, not only in magnetic
Body surface face forms alloy firm layer, and grain boundary decision infiltration can be generated at border, so that the coercivity of magnet obtains obviously
It improves, and can guarantee that the original remanent magnetism of magnet and maximum magnetic energy product do not occur significantly to reduce, avoid in existing method, use
After heavy rare earth compound oxidation, the problem of being not only not achieved and improve coercitive effect, also waste heavy rare earth resource, save
Heavy rare earth resource, reduces costs.The experimental results showed that neodymium iron boron magnetic body provided by the invention, i.e., a kind of compound neodymium iron boron
Magnet, magnet coercivity can improve about 51%, and remanent magnetism and maximum magnetic energy product kept stable, and obvious drop occurs
It is low.
Detailed description of the invention
Fig. 1 is the process flow diagram of the preparation method of neodymium iron boron magnetic body provided by the invention.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
All raw materials of the present invention, are not particularly limited its source, buying on the market or according to those skilled in the art
The preparation of conventional method known to member；All raw materials of the present invention, are not particularly limited its purity, present invention preferably employs
It analyzes pure.
The present invention provides a kind of neodymium iron boron magnetic bodies, including neodymium iron boron magnetic body blank and the RTMH alloy for being compounded in its surface
Layer；
The R is selected from one of rare earth element or a variety of；
The T is Fe and/or Co；
The M be selected from Al, Si, Ti, V, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta,
W, one of Pt, Au, Pb and Bi or a variety of；
The H is protium.
In RTMH alloy of the present invention, the R preferably is selected from one of rare earth element or a variety of, more preferably Sc, Y,
One of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu or a variety of；The T be preferably Fe and/
Or Co, more preferably Fe or Co；The M preferably be selected from Al, Si, Ti, V, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag,
One of In, Sn, Sb, Hf, Ta, W, Pt, Au, Pb and Bi or a variety of, more preferably Al, Ti, Mn, Cu, Ga, Ge, Zr, Mo,
It is a variety of in Ag, In, Sn, Ta, W, Au and Bi；The H is element hydrogen.
The specific ratio of each ingredient in the RTMH alloy is not particularly limited in the present invention, and those skilled in the art can be with
It is selected and is adjusted according to factors such as practical condition, product requirement and quality controls, RTMH alloy of the present invention
In layer, the R is preferably 50~100 parts by weight, more preferably 60~90 parts by weight, most preferably 70~80 parts by weight；The T
Preferably less than or equal to 44 parts by weight, more preferably 5~40 parts by weight, more preferably 10~30 parts by weight, most preferably 15
~25 parts by weight；The M is preferably less than or equal to 49 parts by weight, more preferably 5~45 parts by weight, more preferably 10~40 weights
Measure part, most preferably 15~35 parts by weight；The H is preferably less than or equal to 2 amount parts, more preferably 0.2~1.8 parts by weight,
More preferably 0.5~1.5 parts by weight, most preferably 0.8~1.2 parts by weight.The present invention carrys out H element in the RTMH alloy
Source is not particularly limited, and in a manner of H element is added in alloy well known to those skilled in the art, the present invention is preferably original
Material carries out hydrogen abstraction reaction during hydrogen breaking and introduces H element, by the process of hydrogen abstraction reaction come or dehydrogenation reaction later
Process control the content of H element.The present invention is not special to specific ratio of the RTMH alloy in neodymium iron boron magnetic body
Limitation, those skilled in the art can according to practical condition, product requirement and quality control etc. factors select and
Adjustment, the ratio that the quality of RTMH alloy-layer of the present invention accounts for the neodymium iron boron magnetic body gross mass are preferably less than or equal to
5%, more preferably 1%~4%, more preferably 1.5%~3.5%, most preferably 2%~3%.
The composition of the neodymium iron boron magnetic body blank is not particularly limited in the present invention, with neodymium well known to those skilled in the art
The composition of iron boron magnet blank can be selected according to factors such as practical condition, product requirement and quality controls
It selects and adjusts, each ingredient forms by mass percentage in neodymium iron boron magnetic body blank of the present invention, preferably includes: Pr-Nd:28%
~33%, Dy:0~10%, Tb:0~10%, Nb:0~5%, B:0.5%~2.0%, Al:0~3.0%, Cu:0~1%,
Co:0~3%, Ga:0~2%, Gd:0~2%, Ho:0~2%, Zr:0~2% and surplus Fe, more preferably include Pr-Nd:
28.40%~33.00%, Dy:0.50%~6.0%, Tb:0.50%~6.0%, B:0.92%~0.98%, Al:0.10%
~3.0%, the Fe of Cu:0.10%~0.25%, Co:0.10%~3.0%, Ga:0.1%~0.3% and surplus.Institute of the present invention
The ingredient stated in neodymium iron boron magnetic body blank forms by mass percentage, and it is also preferable to include one of other rare earth elements or more
Kind, more preferably further include one of Sc, Y, La, Ce, Pm, Sm, Eu, Er, Tm, Yb and Lu or a variety of, most preferably Sc and/or
Y.The neodymium iron boron blank is not particularly limited in the present invention, with neodymium iron boron blank well known to those skilled in the art, i.e.,
Neodymium iron boron raw material by ingredient, melting, broken powder, powder orientation compression moulding and vacuum-sintering processed and etc. after neodymium iron boron
Blank, i.e., using surface treatment and processing after, so that it may as common finished product neodymium iron boron magnetic body.
The present invention to it is described it is compound be not particularly limited, with complex method well known to those skilled in the art, this hair
Bright described compound concrete mode be preferably one of brushing, smearing, spraying, cladding, fitting, roll-in, infiltration and dipping or
A variety of, the present invention preferably coats.The compound detailed process is not particularly limited in the present invention, and those skilled in the art can
To be adjusted and select according to practical service environment, product requirement or requirement for anticorrosion, compound preferably process of the present invention
It is compound after heat treatment；The present invention especially limits the heat treatment without other, with neodymium iron boron well known to those skilled in the art
The diffusion heat treatments process of magnet.
The present invention also provides a kind of preparation methods of neodymium iron boron magnetic body, comprising the following steps:
A after) mixing RTMH alloy powder with organic solvent, suspension is obtained；
The R is selected from one of rare earth element or a variety of；The T is Fe and/or Co；The M be selected from Al, Si, Ti, V,
One of Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta, W, Pt, Au, Pb and Bi or a variety of；
The H is protium；
B) suspension for obtaining above-mentioned steps is coated in neodymium iron boron blank surface, obtains semi-finished product；
C after) semi-finished product for obtaining above-mentioned steps are heat-treated, neodymium iron boron magnetic body is obtained.
It is and preceding such as without especially indicating to the range of choice and optimum principle of the raw material in the above-mentioned preparation method of the present invention
The range of choice for stating neodymium iron boron magnetic body is consistent with optimum principle, and this is no longer going to repeat them.
After the present invention first mixes RTMH alloy powder with organic solvent, suspension is obtained.The present invention is to the RTMH
The source of alloy powder is not particularly limited, and prepares in the method well known to those skilled in the art for preparing alloy powder or commercially available
, the present invention preferably obtains after ingredient, melting, hydrogen breaking (inhale hydrogen) by raw material in proportion.According to practical condition, produce
Product require or quality control is selected and adjusted, can uniformly mix and effectively applied to preferred embodiment, institute of the present invention
The average particle size for stating RTMH alloy powder is preferably 1~20 μm, more preferably 2~17 μm, more preferably 2~12 μm, most preferably
It is 2~8 μm.
The organic solvent is not particularly limited in the present invention, those skilled in the art can according to practical service environment,
Product requirement or requirement for anticorrosion are adjusted and select, and organic solvent of the present invention is preferably volatile organic solvent, more
Preferably include one of gasoline, ethyl alcohol and acrylic acid or a variety of, more preferably gasoline, ethyl alcohol or acrylic acid, more preferably vapour
Oil and/or ethyl alcohol, most preferably gasoline or ethyl alcohol.The additional amount of the organic solvent is not particularly limited in the present invention, ability
Field technique personnel can be adjusted according to practical condition, with can be evenly dispersed for preferred embodiment.The present invention is to described
Mixed condition is not particularly limited, and those skilled in the art can be according to practical condition, product requirement or quality control
System is adjusted, and can uniformly mix and be dispersed into suspension as preferred embodiment, the present invention is preferred to the mixed temperature
It is 15~35 DEG C, more preferably 20~30 DEG C, most preferably 23~27 DEG C；It is preferably 7~17 hours to the mixed time,
More preferably 10~15 hours, most preferably 12~13 hours.
The present invention is coated onto neodymium iron boron blank surface, obtains semi-finished product after above-mentioned steps obtain suspension.This
Invention is consistent to the ratio and optimum principle of the neodymium iron boron magnetic body blank and aforementioned neodymium iron boron magnetic body blank, not another herein
One repeats.
The neodymium iron boron blank is not particularly limited in the present invention, is with neodymium iron boron blank well known to those skilled in the art
Can, i.e., neodymium iron boron raw material by ingredient, melting, broken powder, powder orientation compression moulding and vacuum-sintering processed and etc. after
Neodymium iron boron blank, i.e., using surface treatment and processing after, so that it may as common finished product neodymium iron boron magnetic body.The present invention is more preferable
Raising neodymium iron boron magnetic body property, neodymium iron boron blank is further preferably processed as the semi-finished product close to the size of finished product, semi-finished product
It is pre- more preferably on this basis to be carried out oil removing, cleaning etc. by the size for being closely sized to finished product of differently- oriented directivity again for neodymium iron boron blank
Processing, makes its surfacing, cleaning, to reach preferably coating effect.
The coating is not particularly limited in the present invention, with coating processes well known to those skilled in the art, preferably
Including smearing, the modes such as spray, be soaked or dipped, the present invention is preferably impregnated, i.e., is immersed in neodymium iron boron blank described suspended
In liquid, semi-finished product are obtained.The dosage of the coating is not particularly limited in the present invention, and those skilled in the art can be according to reality
The condition of production, product requirement and quality requirement are voluntarily adjusted, and the present invention preferably meets uniformly coating comprehensively.
After the semi-finished product that the present invention again obtains above-mentioned steps are heat-treated, neodymium iron boron magnetic body is obtained.The present invention is to institute
The process and step for stating heat treatment are not particularly limited, with similar process of thermal treatment well known to those skilled in the art,
Present invention preferably comprises High temperature diffusion processing and lonneal processing；The concrete technology that the present invention handles the High temperature diffusion does not have
There is special limitation, with the technique that High temperature diffusion well known to those skilled in the art is handled, the present invention is to ensure the crystalline substance of magnet
Long greatly preferred embodiment does not occur substantially for grain, on this basis it is further preferred that the temperature of High temperature diffusion processing is preferably 700
~1000 DEG C, more preferably 750~950 DEG C, most preferably 800~900 DEG C；The time of the High temperature diffusion processing is preferably 3
~20 hours, more preferably 5~18 hours, more preferably 8~15 hours, most preferably 10~12 hours.The lonneal
Treatment temperature is preferably 350~750 DEG C, more preferably 400~700 DEG C, most preferably 500~600 DEG C；At the lonneal
The time of reason is preferably 1~8 hour, more preferably 2~7 hours, more preferably 3~6 hours, most preferably 4~5 hours.
The other conditions of the heat treatment are not particularly limited in the present invention, with magnet heat well known to those skilled in the art
The condition of processing, the present invention are to improve the effect of heat treatment process, are further preferably first being evacuated to 10 to heat treatment environment- 2Then Pa under protective atmosphere hereinafter, be heat-treated.The equipment of the heat treatment is not particularly limited in the present invention, with this
The equipment of the heat treatment of magnet known to the technical staff of field, the present invention is preferably vacuum sintering furnace, more preferably uses bottom surface
Smooth sintering box more preferably uses on-deformable graphite or C-C plate.
The present invention has obtained neodymium iron boron magnetic body after above-mentioned steps.After the present invention is to above-mentioned steps, may further include
Post-processing step, such as cleaning, slice and etc. be not particularly limited, those skilled in the art can be according to actual production feelings
Condition, product requirement etc. are adjusted or select.Referring to Fig. 1, Fig. 1 is the work of the preparation method of neodymium iron boron magnetic body provided by the invention
Skill general flow chart.
The present invention, by RTMH alloy powder, is coated on neodymium iron boron magnetic body blank surface by diffusion heat using above-mentioned steps
After reason, neodymium iron boron magnetic body has been obtained.RTMH alloy powder is first made into suspension by the present invention, is handled by grain boundary decision infiltration,
I.e. using coating, the modes such as deposition, plating, sputter, cover, so that RTMH alloy powder is first attached to the conduct of magnet outer surface and spread
Source is heat-treated in a certain temperature range, and not only RTMH makes alloy powder be coated on neodymium iron boron magnetic body blank surface, is formed
RTMH alloy-layer, and make the RTMH alloy powder grain boundary diffusion at border to main phase grain surface layer, replace Grain Surface
Nd2Fe14Nd in B forms (Nd, alloy powder)2Fe14B shell structurre improves grain surface anisotropy field, while improving crystalline substance
Boundary's microscopic structure, so that the coercivity of magnet is improved significantly, moreover it is possible to guarantee the original remanent magnetism of magnet and maximum magnetic energy product not
Apparent reduction occurs, after avoiding heavy rare earth compound oxidation, is not only not achieved and improves coercitive effect, also waste weight
The problem of rare earth resources, has saved heavy rare earth resource, has reduced costs.The experimental results showed that neodymium-iron-boron provided by the invention
Body, i.e., a kind of compound neodymium iron boron magnetic body, magnet coercivity can improve about 51%, and remanent magnetism and maximum magnetic energy product are protected substantially
It is fixed to keep steady, and is not substantially reduced.
For a further understanding of the present invention, below with reference to embodiment to provide a kind of neodymium iron boron magnetic body and preparation method thereof into
Row explanation, protection scope of the present invention are not limited by the following examples.
Embodiment 1
RTMH alloy powder is prepared by formula as below:
R is selected from Nd, and T is selected from Fe, and M is selected from Al；In powder the mass percent of Nd, Fe, Al, H be respectively 70%, 15%,
14.5% and 0.5%；Powder mean particle sizes are about 3.0 μm.
The RTMH alloy powder that above-mentioned steps are obtained -- NdFeAlH fine powder is added in ethyl alcohol, forms suspension.
By powder smelting, processed, the 35UH magnet blank of molding, sintering step preparation, being processed as 59*11*1.8, (1.8 be to take
To direction) semi-finished product, semi-finished product are processed, the pretreatments such as oil removing keep its surface cleaning smooth；Then after pre-processing
Semi-finished product be put into suspension impregnate coating, so that its surface is uniformly coated with one layer of NdFeAlH film, coating weight/gross weight
Amount is 3%；Semi-finished product are placed in sintering graphite box again, the graphite for being placed with product is put into sintering furnace, is evacuated to
10-2Pa hereinafter, in argon gas 880 DEG C at a temperature of, carry out level-one be heat-treated 10h, then 510 DEG C at a temperature of, carry out it is low
After temperature tempering second level heat treatment 5h, neodymium iron boron magnetic body is obtained.
Neodymium iron boron magnetic body and common neodymium iron boron magnetic body to the above method of the present invention preparation carry out parallel test comparison, comparison
As a result referring to table 1, table 1 is the magnet performance data for implementing front and back.
Table 1 implements the magnet performance data of front and back
As shown in Table 1, the neodymium iron boron magnetic body of above method preparation of the present invention is than common neodymium iron boron magnetic body in magnet coercivity
Aspect of performance improves about 30%, and remanent magnetism and maximum magnetic energy product aspect of performance kept stable.
Embodiment 2
RTMH alloy powder is prepared by formula as below:
R is selected from Tb, and T is selected from Co, and M is selected from Cu；In powder the mass percent of Tb, Co, Cu, H be respectively 90%, 5.7%,
4% and 0.3%；Powder mean particle sizes are about 3.6 μm.
The RTMH alloy powder that above-mentioned steps are obtained -- TbCoCuH fine powder is added in ethyl alcohol, forms suspension.
By powder smelting, processed, the 48SH magnet blank of molding, sintering step preparation, it is processed as 44.3*21*1.7mm (1.7
For differently- oriented directivity) semi-finished product, semi-finished product are processed, the pretreatments such as oil removing keep its surface cleaning smooth；Then will locate in advance
Semi-finished product after reason, which are put into suspension, impregnates coating, its surface is made uniformly to be coated with one layer of TbCoCuH film, and coating weight/
Total weight is 2%；Semi-finished product are placed in sintering graphite box again, the graphite for being placed with product is put into sintering furnace, are taken out true
Sky is to 10-2Pa hereinafter, in argon gas 850 DEG C at a temperature of, carry out level-one be heat-treated 9h, then 500 DEG C at a temperature of, carry out
After lonneal second level is heat-treated 5h, neodymium iron boron magnetic body is obtained.
Neodymium iron boron magnetic body and common neodymium iron boron magnetic body to the above method of the present invention preparation carry out parallel test comparison, comparison
As a result referring to table 2, table 2 is the magnet performance data for implementing front and back.
Table 2 implements the magnet performance data of front and back
As shown in Table 2, the neodymium iron boron magnetic body of above method preparation of the present invention is than common neodymium iron boron magnetic body in magnet coercivity
Aspect of performance improves about 51%, and remanent magnetism and maximum magnetic energy product aspect of performance kept stable.
Embodiment 3
RTMH alloy powder is prepared by formula as below:
R is selected from Dy, and T is selected from Fe, and M is selected from Cu；In powder the mass percent of Dy, Fe, Cu, H be respectively 60%, 20%,
19% and 1%；Powder mean particle sizes are about 3.2 μm.
The RTMH alloy powder that above-mentioned steps are obtained -- DyFeCuH fine powder is added in ethyl alcohol, forms suspension.
By powder smelting, processed, the 45M magnet blank of molding, sintering step preparation, being processed as 39.5*15.8*2mm, (2 are
Differently- oriented directivity) semi-finished product, semi-finished product are processed, the pretreatments such as oil removing keep its surface cleaning smooth；It then will pretreatment
Semi-finished product afterwards, which are put into suspension, impregnates coating, its surface is made uniformly to be coated with one layer of DyFeCuH film, coating weight/total
Weight is 5%；Semi-finished product are placed in sintering graphite box again, the graphite for being placed with product is put into sintering furnace, is vacuumized
To 10-2Pa hereinafter, in argon gas 820 DEG C at a temperature of, carry out level-one be heat-treated 10h, then 510 DEG C at a temperature of, carry out
After lonneal second level is heat-treated 4h, neodymium iron boron magnetic body is obtained.
Neodymium iron boron magnetic body and common neodymium iron boron magnetic body to the above method of the present invention preparation carry out parallel test comparison, comparison
As a result referring to table 3, table 3 is the magnet performance data for implementing front and back.
Table 3 implements the magnet performance data of front and back
As shown in Table 3, the neodymium iron boron magnetic body of above method preparation of the present invention is than common neodymium iron boron magnetic body in magnet coercivity
Aspect of performance improves about 44%, and remanent magnetism and maximum magnetic energy product aspect of performance kept stable.
A kind of neodymium iron boron magnetic body provided by the present invention and preparation method thereof is described in detail above.It answers herein
With a specific example, principle and implementation of the present invention are described, and the explanation of above example is only intended to help
Understand method and its core concept of the invention.It should be pointed out that for those skilled in the art, not taking off
, can be with several improvements and modifications are made to the present invention under the premise of from the principle of the invention, these improvement and modification also fall into this
In invention scope of protection of the claims.
Claims (2)
1. a kind of neodymium iron boron magnetic body, which is characterized in that including neodymium iron boron magnetic body blank and the RTMH alloy-layer for being compounded in its surface；
The neodymium iron boron magnetic body is the magnet product after heat treatment；
The neodymium iron boron magnetic body is compound neodymium iron boron magnetic body, is had at the border of the neodymium iron boron magnetic body blank and RTMH alloy-layer
There is scattering and permeating layer；
The R is selected from one of rare earth element or a variety of；
The T is Fe and/or Co；
The M be selected from Al, Si, Ti, V, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta, W, Pt,
One of Au, Pb and Bi or a variety of；
The H is protium；
The ratio that the quality of the RTMH alloy-layer accounts for the neodymium iron boron magnetic body gross mass is less than or equal to 5%；
Include: in the RTMH alloy-layer
50~100 parts by weight of R；
T is less than or equal to 44 parts by weight；
M is less than or equal to 49 parts by weight；
H is less than or equal to 2 parts by weight；
Each ingredient forms by mass percentage in the neodymium iron boron magnetic body blank, comprising: Pr-Nd:28%~33%；Dy:0~
10%；Tb:0~10%；Nb:0~5%；B:0.5%~2.0%；Al:0~3.0%；Cu:0~1%；Co:0~3%；Ga:0
~2%；Gd:0~2%；Ho:0~2%；Zr:0~2%；Surplus is Fe；
It further include one of other rare earth elements or a variety of in the ingredient of the neodymium iron boron magnetic body blank.
2. a kind of preparation method of neodymium iron boron magnetic body as described in claim 1, comprising the following steps:
A after) mixing RTMH alloy powder with organic solvent, suspension is obtained；
The R is selected from one of rare earth element or a variety of；The T is Fe and/or Co；The M be selected from Al, Si, Ti, V, Cr,
One of Mn, Ni, Cu, Zn, Ga, Ge, Zr, Nb, Mo, Ag, In, Sn, Sb, Hf, Ta, W, Pt, Au, Pb and Bi or a variety of；Institute
Stating H is protium；
B) suspension for obtaining above-mentioned steps is coated in neodymium iron boron blank surface, obtains semi-finished product；
C after) semi-finished product for obtaining above-mentioned steps are heat-treated, neodymium iron boron magnetic body is obtained；
The average particle size of the RTMH alloy powder is 1~20 μm；The organic solvent includes in gasoline, ethyl alcohol and acrylic acid
It is one or more；
The mixed temperature is 15~35 DEG C, and the mixed time is 7~17 hours；
The heat treatment includes High temperature diffusion processing and lonneal processing；
The temperature of the High temperature diffusion processing is 700~1000 DEG C, and the time of the High temperature diffusion processing is 3~20 hours；
The temperature of the lonneal processing is 350~750 DEG C, and the time of the lonneal processing is 1~8 hour.
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| CN201610305312.2A CN105761861B (en) | 2016-05-10 | 2016-05-10 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| EP16185333.8A EP3182423B1 (en) | 2015-12-18 | 2016-08-23 | Neodymium iron boron magnet and preparation method thereof |
| US15/268,725 US9947447B2 (en) | 2015-12-18 | 2016-09-19 | Neodymium iron boron magnet and preparation method thereof |
| JP2016190585A JP6606044B2 (en) | 2015-12-18 | 2016-09-29 | Neodymium iron boron magnet and method for preparing the same |
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| CN106601462A (en) * | 2016-12-14 | 2017-04-26 | 中国工程物理研究院材料研究所 | Surface crystal boundary modification method for improving corrosion resistance of sintered Nd-Fe-B magnet and product prepared by method |
| CN107492430A (en) * | 2017-08-09 | 2017-12-19 | 江西金力永磁科技股份有限公司 | A kind of neodymium iron boron magnetic body and preparation method thereof |
| CN107492432B (en) * | 2017-08-15 | 2019-10-18 | 宁波合力磁材技术有限公司 | A kind of preparation method of Nd-Fe-B permanent magnet |
| KR102398932B1 (en) | 2018-08-31 | 2022-05-16 | 주식회사 엘지화학 | Method for preparing magnetic material and magnetic material |
| CN109585111A (en) * | 2018-11-19 | 2019-04-05 | 浙江东阳东磁稀土有限公司 | A kind of preparation method of no dysprosium terbium high-performance permanent magnet |
| CN109509630B (en) * | 2019-01-15 | 2020-08-14 | 内蒙古北方众恒磁谷新材料有限公司 | Sintered Nd-Fe-B permanent magnet manufacturing process for magnetic jack |
| CN110911150B (en) | 2019-11-28 | 2021-08-06 | 烟台首钢磁性材料股份有限公司 | Method for improving coercive force of neodymium iron boron sintered permanent magnet |
| CN112700939A (en) * | 2020-12-06 | 2021-04-23 | 江西金力永磁科技股份有限公司 | Composite neodymium-iron-boron magnet and preparation method thereof |
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| JP2005011973A (en) * | 2003-06-18 | 2005-01-13 | Japan Science & Technology Agency | Rare earth-iron-boron based magnet and its manufacturing method |
| JP4656323B2 (en) * | 2006-04-14 | 2011-03-23 | 信越化学工業株式会社 | Method for producing rare earth permanent magnet material |
| JP5328161B2 (en) * | 2008-01-11 | 2013-10-30 | インターメタリックス株式会社 | Manufacturing method of NdFeB sintered magnet and NdFeB sintered magnet |
| JP5284394B2 (en) * | 2011-03-10 | 2013-09-11 | 株式会社豊田中央研究所 | Rare earth magnet and manufacturing method thereof |
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