CN106876072A - The method for improving neodymium-iron-boron magnetic material magnetic property - Google Patents
The method for improving neodymium-iron-boron magnetic material magnetic property Download PDFInfo
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- CN106876072A CN106876072A CN201510922166.3A CN201510922166A CN106876072A CN 106876072 A CN106876072 A CN 106876072A CN 201510922166 A CN201510922166 A CN 201510922166A CN 106876072 A CN106876072 A CN 106876072A
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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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
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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
- H01F1/0572—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 with a protective layer
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Abstract
The invention discloses a kind of method for improving neodymium-iron-boron magnetic material magnetic property, it includes：Using the anhydrous organic suspension liquid of rare earth compound powder as electrophoresis solution, and to pass through the Sintered NdFeB magnet for pre-processing as negative electrode, rare earth compound is deposited on the magnet by electrophoretic deposition method, so as to form the rare earth compound coating of flat even in the magnet surface, wherein the rare earth compound is selected from rare earth fluoride and/or rare earth oxide；And, the magnet to surface with the rare earth compound coating is dried treatment, diffusion heat treatments and temper successively.The thickness of the rare earth compound coating of deposition can be effectively controlled by present invention process, deposition process is fast, and deposition efficiency is high, and through the magnet after treatment on the premise of remanent magnetism is basically unchanged, coercivity is significantly improved, increase rate is up to 2~9kOe.Present invention process process is simply controllable simultaneously, and rare earth utilization rate is high, has huge advantage in technical scale metaplasia product.
Description
Technical field
The invention belongs to field of magnetic material, and in particular to a kind of method of raising neodymium-iron-boron magnetic material magnetic property.
Background technology
The neodymium iron boron magnetic body of the title with " magnetic king " is widely used to every field with its excellent magnetic property.In recent years, with
The rise of hybrid vehicle, pure electric automobile, wind-power electricity generation, active demand has the magnet of more high-coercive force (Hcj).Mesh
Before, improving the coercivity of sintered NdFeB magnet mainly has crystal grain thinning and addition two kinds of approach of heavy rare earth element, wherein using molten
It is generally to use at present that refining or dual alloy method add heavy rare earth element (HRE), and a kind of very effective means, but is used
This method exists following not enough：One is due to 2:14:In 1 phase, heavy rare earth element Dy or Tb and Fe forms antiferromagnetic coupling
Close, the saturation magnetization (Ms) of magnet compares Nd2Fe14B phases are low, so as to cause the remanent magnetism (Br) of magnet and magnetic energy product ((BH) max)
Reduce；Two is the heavy rare earth element scarcity of resources such as Dy, Tb, expensive, and excessive heavy rare earth element, meeting are added in production
The production cost of magnet is caused to improve.Therefore reducing the heavy rare earth element usage amount of high-coercive force neodymium iron boron magnetic body turns into current domestic
The focus and emphasis of international research.
In recent years, grain boundary decision method is considered as that one kind can significantly improve magnet coercivity on the premise of magnet remanent magnetism is not influenceed
Very effective method.Heavy rare earth element is expanded from magnet surface along crystal boundary in heat treatment process using the method for grain boundary decision
It is scattered to inside magnet, heavy rare earth element is primarily present in the periphery of crystal boundary and crystal grain without excessive entrance intra-die, is formed
(Nd, HRE)2Fe14The shell structurre of B phases, so as to significantly improve the coercivity of magnet and keep remanent magnetism constant.At present,
Through reporting various grain boundary diffusion process rare earth element being diffused into from magnet surface inside magnet.For example, one kind is by splashing
The method penetrated or be deposited with, sintered NdFeB magnet surface is deposited on by rare earth elements such as Dy, Pr, Tb, is then diffused heat
Treatment；Another kind is to coat rare earth compound such as fluoride powder and the technique for carrying out diffusion heat treatments in magnet surface.Another
It is to deposit the one layer of heavy rare earth compound of aqueous molecule (such as hydrated basic nitric acid (carbonic acid) in magnet surface using ability cathode electrophoresis
Rare-earth salts), then it is diffused heat treatment.Rare earth element can be made along crystal boundary and main phase grain surface region by the above method
Infiltration, make rare earth element be primarily present in crystal grain periphery without excessive entrance magnet inside, not only increase coercivity, also
The usage amount of expensive heavy rare earth has been saved to a certain extent, and remanent magnetism and magnetic energy product are not substantially reduced.But these methods exist
There are still many weak points in actual application：(1) evaporation process coating thickness is difficult to control, and largely weighs dilute
Earth metal is dispersed in heating furnace chamber room, causes the unnecessary waste of heavy rare earth metal, and utilization rate is low；(2) sputtering method will
, in sintered NdFeB magnet surface, vacuum requirement degree is high, and sputtering yield is low, and apparatus expensive, operation is taken for Dy or Tb metal deposits
With too high, it is not suitable for production application；(3) the fluoride powder of Dy or Tb is attached to sintered NdFeB magnetic by cladding process
Body surface face, method is simple, but adhesion layer is uneven, and thickness is uncontrollable, causes homogeneity of product poor, it is difficult to realize
Industrialization.It is coercitive to improve limited if coating is too thin, and coating is too thick, can cause the waste of heavy rare earth element；(4)
Rare earth compound magnet surface be can be deposited to using ability cathode electrophoresis, uniform ground, the weight that thickness is controllable, adhesive force is good obtained
Rare earth coating, but hydrated basic nitric acid (carbonic acid) rare-earth salts for wherein using is being configured to the colloidal solution process and Re Chu of powder
During reason, can produce such as NO3 -、OH-、H2O etc. is easy to ion or the change reacted with neodymium iron boron magnetic body rare earth elements
Compound, easily produces corrosion to magnet, so as to the structure and performance to magnet are adversely affected.
The content of the invention
It is a primary object of the present invention to provide a kind of method for improving neodymium-iron-boron magnetic material magnetic property, to overcome in the prior art
Deficiency.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
The embodiment provides a kind of method for improving neodymium-iron-boron magnetic material magnetic property, it includes：
Anhydrous organic suspension liquid using rare earth compound powder is used as electrophoresis solution, and the Sintered NdFeB magnet pre-processed with process
As negative electrode, rare earth compound is deposited on the magnet by electrophoretic deposition method, so as to form flat in the magnet surface
Smooth uniform rare earth compound coating, wherein the rare earth compound is selected from rare earth fluoride and/or rare earth oxide；
And, the magnet to surface with the rare earth compound coating is dried treatment, diffusion heat treatments and returns successively
Fire treatment.
Further, the rare earth compound preferably from fluorination terbium, dysprosium fluoride, praseodymium fluoride, the rare earth fluoride such as neodymium fluoride and
Any one in the rare earth oxides such as terbium oxide, dysprosia, praseodymium oxide, neodymia or two or more combinations.
More preferred, the concentration of contained rare earth compound powder is 2~30g/L in the electrophoresis solution.
More preferred, the granularity of the rare earth compound powder is 50nm~50 μm.
In some preferred embodiments, the condition that the electrophoretic deposition method is used includes：Deposition voltage is 20~90V, deposition
Time is 10s~10min；And/or, the distance between electrode is 20~100mm.
More preferred, the thickness of the rare earth compound coating is 10~150 μm.
In some preferred embodiments, the condition that the dried process is used includes：Temperature is 60~120 DEG C, and the time is 20
Min~24h.
In some preferred embodiments, the diffusion heat treatments are to be less than 10 in inert atmosphere or vacuum-3The vacuum environment of Pa
In carry out, and the heat treatment temperature for using is 700~1000 DEG C, and soaking time is 0.5~15h, is cooled down afterwards.
In some preferred embodiments, the temper is to be less than 10 in inert atmosphere or vacuum-3In the vacuum environment of Pa
Carry out, and the temperature for using is 460~560 DEG C, soaking time is 0.5~10h, is cooled down afterwards.
Further, the mode of the cooling may be selected from air-cooled or water-cooled, but not limited to this.
Further, in the method for improving neodymium-iron-boron magnetic material magnetic property, Sintered NdFeB magnet is pre-processed
Process can include：Sintered NdFeB magnet is placed in the solution containing degreaser the greasy dirt for removing magnet surface, then with ultrasound
Ripple is washed to magnet surface free from admixture, then is cleaned neodymium iron boron magnetic body 3~4 times with absolute ethyl alcohol etc..
Present invention process is using the suspension of rare earth compound powder as electrophoresis solution, and the sintered NdFeB magnetic pre-processed with process
These rare earth compounds are deposited to the magnet surface by body as substrate (negative electrode) using electrophoretic deposition method, wherein by control
The electrophoretic parameters such as electrophoretic deposition voltage processed, sedimentation time, electrode spacing the magnet surface obtain flat even, thickness it is controllable,
The good rare earth compound coating of adhesive force, is then carried out successively by the magnet by surface with the rare earth compound coating
Dry, diffusion heat treatments and temper, make heavy rare earth element enter inside the magnet along crystal boundary, and be enriched in main phase grain
Periphery and form shell structurre, and then the coercivity of sintered Nd-Fe-B permanent magnetic material is increased dramatically.
Compared with prior art, advantages of the present invention includes：
(1) rare earth compound coating is prepared using electrophoretic deposition in the technique for providing, can effectively controls the rare earth chemical combination of deposition
The thickness of thing coating, deposition process is fast, and deposition efficiency is high, it is possible in the Sintered NdFeB magnet table of complicated, arbitrary shape
Face is formed has the controllable rare earth compound coating of the uniform, smooth of preferable adhesion, thickness with neodymium iron boron magnetic body, realizes optimal
Rare earth content additive effect, so as to realize the efficient utilization of heavy rare earth, while not chemically reacted in electrophoretic deposition process, sinks
Remaining suspension may continue to Collection utilization after product, so as to effectively increase the utilization rate of rare earth compound raw material, it is to avoid
Waste of the heavy rare earth metal in coating preparation process, is appropriate for large-scale industrial production；
(2) technique for providing is after electrophoretic deposition forms rare earth compound coating, then is processed by High temperature diffusion, makes to be deposited on
The rare earth compound of magnet surface from magnet surface grain boundary diffusion to magnet inside, and crystal grain periphery formed shell structurre, from
And the coercivity of magnet in the case where magnet remanent magnetism is not reduced, can be made to be significantly increased (for example, 2~9 can be improved compared with before processing
KOe, amplification about 12~57%).
Brief description of the drawings
In order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art, below will be to embodiment or prior art
The accompanying drawing to be used needed for description is briefly described, it should be apparent that, drawings in the following description are only note in the application
Some embodiments for carrying, for those of ordinary skill in the art, on the premise of not paying creative work, can be with root
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 a are the Sintered NdFeB magnet electrophoretic deposition dysprosium fluoride of embodiment 1 front and rear under Different Heat Treatment Conditions, the demagnetization of sample
Curve map；
Fig. 1 b are the variation relation figure of the coercivity diffusion heat treatments temperature of sample after the electrophoretic deposition dysprosium fluoride of embodiment 1；
Fig. 1 c be the electrophoretic deposition dysprosium fluoride of embodiment 1 after sample remanent magnetism with diffusion heat treatments temperature variation relation figure；
Fig. 1 d be the electrophoretic deposition dysprosium fluoride of embodiment 1 after sample maximum magnetic energy product with diffusion heat treatments temperature variation relation figure；
Fig. 2 a are the magnetism testing figure before the Sintered NdFeB magnet electrophoretic deposition of embodiment 2 fluorination terbium；
Fig. 2 b are the magnetism testing figure after the Sintered NdFeB magnet electrophoretic deposition of embodiment 2 fluorination terbium；
Fig. 3 a are the magnetism testing figure before the Sintered NdFeB magnet electrophoretic deposition dysprosia of embodiment 3；
Fig. 3 b are the magnetism testing figure after the Sintered NdFeB magnet electrophoretic deposition dysprosia of embodiment 3.
Specific embodiment
In view of many defects of prior art, inventor is able to propose technology of the invention through studying for a long period of time and largely putting into practice
Scheme, it relates generally to a kind of method for improving neodymium-iron-boron magnetic material magnetic property.The method includes：With rare earth compound RX
The anhydrous organic suspension liquid of powder as electrophoresis solution, using by the Sintered NdFeB magnet of pretreatment as substrate (negative electrode), and
The rare earth compound is deposited into the magnet surface using electrophoretic deposition method, during by controlling electrophoretic deposition voltage, deposition
Between, the technological parameter such as electrode spacing obtain flat even, the rare earth compound that thickness is controllable, adhesive force is good in the magnet surface
Coating, then the magnet by surface with the rare earth compound coating be dried successively, at diffusion heat treatments and tempering
Reason, it is final to obtain the sintered Nd-Fe-B permanent magnetic material that coercivity gets a promotion.
It is more preferred, the rare earth compound RX be rare earth fluoride (such as fluorination terbium, dysprosium fluoride, praseodymium fluoride, neodymium fluoride),
One or more in rare earth oxide (such as terbium oxide, dysprosia, praseodymium oxide, neodymia).
In some preferred embodiment, the preparation method of the rare earth compound RX powder suspensions is：By rare earth compound powder
Ultrasonic agitation is into suspension in anhydrous organic solvent (such as ethanol, acetone, preferred alcohol).The rare earth compound powder
Concentration in the suspension is preferably 2~30g/L.
More preferred, the rare earth compound RX powders are the powder of granularity 50nm~50 μm.
It is more preferred, in the method for improving neodymium-iron-boron magnetic material magnetic property, the deposition voltage that electrophoretic deposition process is used
It is 20~90V, sedimentation time is 10s~10min.
More preferred, the magnet surface rare earth compound coating layer thickness is 10~150 μm.
It is more preferred, in the method for improving neodymium-iron-boron magnetic material magnetic property, described rare earth compound is applied to being attached with
The magnet of layer is dried processing method and is：Baking temperature is 60~120 DEG C, and drying time is 20min~24h.
It is more preferred, in the method for improving neodymium-iron-boron magnetic material magnetic property, by with the rare earth compound coating
Magnet is diffused heat treatment method：Neodymium iron boron magnetic body is placed in sintering furnace, 700~1000 DEG C of temperature, soaking time 0.5~15
h.Furnace interior is inert gas, such as argon gas, or is vacuumized, and vacuum is less than 10-3Pa.The type of cooling is air-cooled or water-cooled.
It is more preferred, in the method for improving neodymium-iron-boron magnetic material magnetic property, by with the rare earth compound coating
Magnet carries out tempering method for treating：Neodymium iron boron magnetic body is placed in sintering furnace, 460~560 DEG C of temperature, 0.5~10h of soaking time.
Furnace interior is inert gas, such as argon gas, or is vacuumized, and vacuum is less than 10-3Pa.The type of cooling is air-cooled or water-cooled.
The present invention uses electrophoretic deposition prepares coating, and in electrophoretic deposition process, powered powder particle is dispersed or suspended in
In liquid medium, in the presence of applying direct current electric field, it is attracted and is deposited in the conductive substrates with opposite charges.With it is existing
The grain boundary decision prepares coating method such as some sputterings, coating is compared, and the electrophoretic deposition can at normal temperatures and pressures, in complexity
, the deposition that rare earth compound (such as oxide, fluoride) is realized on the matrix of arbitrary shape, equipment is simple, low cost,
Deposition process is fast, can realize the efficient utilization of rare earth element, it is easy to accomplish large-scale industrial production, and the coating tool for preparing
There is the features such as uniform, smooth, thickness is controllable, the adhesion with matrix is good.
, using rare earth fluoride and rare earth oxide etc. as diffusion source, these compounds are in electrophoretic deposition, heat treated for the present invention
Will not be hydrolyzed in journey or ionized, will not produce the ion for having corrosiveness to magnet, and formed after fluorine/oxygen etc. enters magnet
Nd (- O)-F phases, can suppress the formation for not having contributive HRE-Nd-O phases to coercivity lifting, increase rare earth element in principal phase
In content, so as to lift the utilization ratio of rare earth, meanwhile, heavy rare earth can form shell structurre after being diffused into magnet inside, i.e.,
Main phase grain periphery forms (RE/HRE)2Fe14B phases, make magnet coercivity get a promotion.
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the accompanying drawings to specific embodiment of the invention
It is described in detail.The example of these preferred embodiments is illustrated in the accompanying drawings.Describe shown in accompanying drawing and with reference to the accompanying drawings
Embodiments of the present invention be merely exemplary that and the present invention is not limited to these implementation methods.
Here, also, it should be noted that in order to avoid having obscured the present invention because of unnecessary details, only showing in the accompanying drawings
The structure and/or process step closely related with scheme of the invention, and eliminate that little with relation of the present invention other are thin
Section.
Embodiment 1：Electrophoretic deposition dysprosium fluoride improves Sintered NdFeB magnet magnetic property.
1. take the dysprosium fluoride powder that average granularity is 10 μm to be put into absolute ethyl alcohol, ultrasonic agitation 25min, form suspension, its
Concentration of the middle dysprosium fluoride powder in suspension is 12g/L.
2. Sintered NdFeB magnet is placed in the solution containing degreaser the greasy dirt for removing magnet surface, then with ultrasonic wave water washing extremely
Magnet surface free from admixture, then cleaned neodymium iron boron magnetic body 3~4 times with absolute ethyl alcohol.Then magnet is fixed on electrophoretic deposition set
Negative electrode, immersion suspension in.
3. electrophoretic deposition 8min is carried out under 40V voltages at room temperature, one layer of uniform, smooth fluorine is obtained on neodymium iron boron magnetic body surface
Change dysprosium coating, neodymium iron boron magnetic body is put into 60 DEG C of baking 4h in baking oven by about 100 μm of coating layer thickness afterwards.
4. the neodymium iron boron magnetic body that surface attachment has dysprosium fluoride coating is placed in vacuum sintering furnace and is diffused treatment, vacuum is
5×10-3Pa, 10h is incubated at 700~950 DEG C, treats that temperature is cooled to 80 DEG C, then through 500 DEG C of temper 2h.Obtain magnetic
The Sintered NdFeB magnet of lifting can be obtained.
5. according to GB/T3217-1992 standards (magnetism testing in the present invention is in accordance with this standard) test sintered NdFeB magnetic
The magnetic property of body, is as a result listed in table 1.The sample of wherein comparative example 1 is to be provided without the treated magnet of electrophoretic deposition method.Can be with
Find out, the magnet coercivity of different diffusion temperature treatment reaches 18.35~22.83kOe after electrophoretic deposition, is improved compared with comparative example 1
2.25~6.73kOe, remanent magnetism slightly has reduction, the range of decrease only 0.25~0.48kGs.
It can be seen that, using the method for the present embodiment, one layer of uniform flat, thickness can be deposited on Sintered NdFeB magnet surface
Controllable dysprosium fluoride coating, after diffusion heat treatments and temper, magnet magnetic property is improved, and remanent magnetism slightly has reduction, but
Coercivity and magnetic energy product are substantially improved.
Embodiment 2：Electrophoretic deposition fluorination terbium improves Sintered NdFeB magnet magnetic property.
1. average granularity is taken for the fluorination terbium powder of 50nm or so is put into absolute ethyl alcohol, and ultrasonic agitation 20min is allowed to form outstanding
Supernatant liquid, wherein concentration of the fluorination terbium powder in suspension is 3g/L.
2. Sintered NdFeB magnet is placed in the solution containing degreaser the greasy dirt for removing magnet surface, then with ultrasonic wave water washing extremely
Magnet surface free from admixture, then cleaned neodymium iron boron magnetic body 3~4 times with absolute ethyl alcohol.Then magnet is fixed on electrophoretic deposition set
Negative electrode, immersion suspension in.
3. electrophoretic deposition 5min is carried out under 90V voltages at room temperature, neodymium iron boron magnetic body surface obtain one layer it is uniform, smooth
Neodymium iron boron magnetic body is put into 80 DEG C of baking 24h in baking oven by fluorination terbium coating, about 140 μm of coating layer thickness afterwards.
4. the neodymium iron boron magnetic body that surface attachment has dysprosium fluoride coating is placed in vacuum sintering furnace and is diffused treatment, vacuum is
5×10-3Pa, 8h is incubated at 920 DEG C, treats that temperature is cooled to 80 DEG C, then through 550 DEG C of temper 1h.Obtain magnetic property acquisition
The Sintered NdFeB magnet of lifting.
5. according to GB/T3217-1992 standards (magnetism testing in the present invention is in accordance with this standard) test sintered NdFeB magnetic
The magnetic property of body, as a result shows that the coercivity of the magnet that the embodiment is obtained improves 8.86kOe, and remanent magnetism is in a slight decrease, reduces
0.75kGs；It is as shown in table 2 using magnet performance change after the inventive method before processing.Wherein the sample of comparative example 2 is to be provided without
The treated magnet of electrophoretic deposition method.
It can be seen that, using the method for the present embodiment, one layer of uniform flat, thickness can be deposited on Sintered NdFeB magnet surface
Controllable fluorination terbium coating, after diffusion heat treatments and temper, magnet magnetic property is improved, and remanent magnetism slightly has reduction, but
Coercivity and magnetic energy product are substantially improved.
Embodiment 3：Electrophoretic deposition dysprosia improves Sintered NdFeB magnet magnetic property.
1. take the dysprosia powder that average granularity is 50 μm or so to be put into absolute ethyl alcohol, ultrasonic agitation 35min is allowed to form outstanding
Supernatant liquid, wherein concentration of the fluorination terbium powder in suspension is 30g/L.
2. Sintered NdFeB magnet is placed in the solution containing degreaser the greasy dirt for removing magnet surface, then with ultrasonic wave water washing extremely
Magnet surface free from admixture, then cleaned neodymium iron boron magnetic body 3~4 times with absolute ethyl alcohol.Then magnet is fixed on electrophoretic deposition set
Negative electrode, immersion suspension in.
3. electrophoretic deposition 2min is carried out under 30V voltages at room temperature, neodymium iron boron magnetic body surface obtain one layer it is uniform, smooth
Neodymium iron boron magnetic body is put into 120 DEG C of baking 40min in baking oven by dysprosia coating, about 40 μm of coating layer thickness afterwards.
4. the neodymium iron boron magnetic body that surface attachment has dysprosia coating is placed in vacuum sintering furnace and is diffused treatment, vacuum is
5×10-3Pa, 15h is incubated at 950 DEG C, treats that temperature is cooled to 80 DEG C, then through 470 DEG C of temper 8h.Obtain magnetic property acquisition
The Sintered NdFeB magnet of lifting.
5. according to GB/T3217-1992 standards (magnetism testing in the present invention is in accordance with this standard) test sintered NdFeB magnetic
The magnetic property of body, as a result shows that the coercivity of the magnet that the embodiment is obtained improves 3.01kOe, and remanent magnetism is not changed in substantially, only
Reduce 0.09kGs；It is as shown in table 3 using magnet performance change after the inventive method before processing.The sample of wherein comparative example 3 is
It is provided without the treated magnet of electrophoretic deposition method.
It can be seen that, using the method for the present embodiment, one layer of uniform flat, thickness can be deposited on Sintered NdFeB magnet surface
Controllable dysprosia coating, after diffusion heat treatments and temper, magnet magnetic property is improved, and remanent magnetism slightly has reduction, but
Coercivity and magnetic energy product are substantially improved.
In the embodiment 1 of table 1 before and after Sintered NdFeB magnet electrophoretic deposition Different Heat Treatment Conditions magnetic property
Magnetic property in the embodiment 2 of table 2 before and after Sintered NdFeB magnet electrophoretic deposition fluorination terbium
| Numbering | Magnet specification | Coercivity (kOe) | Remanent magnetism (kGs) | Maximum magnetic energy product (MGOe) |
| Comparative example 2 | Φ10*3mm | 15.59 | 13.63 | 45.23 |
| Embodiment 2 | Φ10*3mm | 24.45 | 12.88 | 40.15 |
Magnetic property in the embodiment 3 of table 3 before and after Sintered NdFeB magnet electrophoretic deposition dysprosia
| Numbering | Magnet specification | Coercivity (kOe) | Remanent magnetism (kGs) | Maximum magnetic energy product (MGOe) |
| Comparative example 3 | Φ10*3mm | 16.10 | 13.17 | 42.92 |
| Embodiment 3 | Φ10*3mm | 19.11 | 13.08 | 42.99 |
Finally, in addition it is also necessary to explanation, term " including ", "comprising" or its any other variant be intended to nonexcludability
Comprising so that process, method, article or equipment including a series of key elements not only include those key elements, but also wrapping
Other key elements being not expressly set out are included, or it is this process, method, article or the intrinsic key element of equipment also to include.
It should be appreciated that above-described embodiment is only explanation technology design of the invention and feature, technique is familiar with its object is to allow
Personage will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all according to this hair
The equivalent change or modification that bright Spirit Essence is made, should all be included within the scope of the present invention.
Claims (10)
1. it is a kind of improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that including：
Anhydrous organic suspension liquid using rare earth compound powder is used as electrophoresis solution, and the Sintered NdFeB magnet pre-processed with process
As negative electrode, rare earth compound is deposited on the magnet by electrophoretic deposition method, so as to form flat in the magnet surface
Smooth uniform rare earth compound coating, wherein the rare earth compound is selected from rare earth fluoride and/or rare earth oxide；
And, the magnet to surface with the rare earth compound coating is dried treatment, diffusion heat treatments and returns successively
Fire treatment.
2. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that：The rare earth
Compound is selected from fluorination terbium, dysprosium fluoride, praseodymium fluoride, neodymium fluoride, terbium oxide, dysprosia, praseodymium oxide, any one in neodymia
Plant or two or more combinations.
3. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that：The electrophoresis is molten
The concentration of contained rare earth compound powder is 2~30g/L in liquid, and the granularity of the rare earth compound powder is 50nm~50 μm.
4. according to claim 1 or 3 raising neodymium-iron-boron magnetic material magnetic property method, it is characterised in that：The electrophoresis
The anhydrous organic solvent used in solution includes ethanol or acetone.
5. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that：The electrophoresis sinks
The condition that product method is used includes：Deposition voltage is 20~90V, and sedimentation time is 10s~10min；And/or, between electrode
Distance is 20~100mm.
6. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that：The rare earth
The thickness of compound coating is 10~150 μm.
7. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that including：It is described dry
The condition that dry treatment is used includes：Temperature is 60~120 DEG C, and the time is 20min~24h.
8. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that including：The expansion
Radiating treatment is to be less than 10 in inert atmosphere or vacuum-3Carried out in the vacuum environment of Pa, and the heat treatment temperature for using for
700~1000 DEG C, soaking time is 0.5~15h, is cooled down afterwards.
9. it is according to claim 1 improve neodymium-iron-boron magnetic material magnetic property method, it is characterised in that including：Described time
Fire treatment is to be less than 10 in inert atmosphere or vacuum-3Carried out in the vacuum environment of Pa, and the temperature for using for 460~
560 DEG C, soaking time is 0.5~10h, is cooled down afterwards.
10. according to claim 8 or claim 9 raising neodymium-iron-boron magnetic material magnetic property method, it is characterised in that：It is described cold
But mode is selected from air-cooled or water-cooled.
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| CN108109833A (en) * | 2017-12-20 | 2018-06-01 | 赣州新瑞迪奥磁性材料有限公司 | A kind of method that high-performance rare-earth permanent-magnetic body is produced by grain boundary decision method |
| CN108565088A (en) * | 2018-05-25 | 2018-09-21 | 严高林 | A kind of band coating sintered NdFeB magnet and preparation method thereof |
| CN109256274A (en) * | 2017-07-14 | 2019-01-22 | 中国科学院宁波材料技术与工程研究所 | The preparation method of low heavy rare earth high-coercive force neodymium iron boron magnetic body |
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| CN110444381A (en) * | 2018-05-04 | 2019-11-12 | 中国科学院宁波材料技术与工程研究所 | A kind of high-performance grain boundary decision neodymium iron boron magnetic body and preparation method thereof |
| CN113130199A (en) * | 2021-04-20 | 2021-07-16 | 中国计量大学 | High-resistivity sintered samarium-cobalt magnet and preparation method thereof |
| CN113403620A (en) * | 2021-06-23 | 2021-09-17 | 中国科学院宁波材料技术与工程研究所 | Rare earth permanent magnet with anticorrosive coating and preparation method and application thereof |
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| CN108109833A (en) * | 2017-12-20 | 2018-06-01 | 赣州新瑞迪奥磁性材料有限公司 | A kind of method that high-performance rare-earth permanent-magnetic body is produced by grain boundary decision method |
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| CN108565088A (en) * | 2018-05-25 | 2018-09-21 | 严高林 | A kind of band coating sintered NdFeB magnet and preparation method thereof |
| CN108565088B (en) * | 2018-05-25 | 2019-08-30 | 严高林 | A kind of band coating sintered NdFeB magnet and preparation method thereof |
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| CN113130199A (en) * | 2021-04-20 | 2021-07-16 | 中国计量大学 | High-resistivity sintered samarium-cobalt magnet and preparation method thereof |
| CN113130199B (en) * | 2021-04-20 | 2022-11-11 | 中国计量大学 | High-resistivity sintered samarium-cobalt magnet and preparation method thereof |
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Application publication date: 20170620 |