CN105679479B - The preparation method of permanent-magnet material and permanent-magnet material - Google Patents
The preparation method of permanent-magnet material and permanent-magnet material Download PDFInfo
- Publication number
- CN105679479B CN105679479B CN201410670051.5A CN201410670051A CN105679479B CN 105679479 B CN105679479 B CN 105679479B CN 201410670051 A CN201410670051 A CN 201410670051A CN 105679479 B CN105679479 B CN 105679479B
- Authority
- CN
- China
- Prior art keywords
- permanent
- magnet material
- magnet
- grain
- size
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 129
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 34
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 11
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 45
- 230000006835 compression Effects 0.000 claims description 34
- 238000007906 compression Methods 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 30
- 238000012545 processing Methods 0.000 claims description 20
- 238000010791 quenching Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 230000000171 quenching effect Effects 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- 230000005389 magnetism Effects 0.000 claims description 8
- 238000007731 hot pressing Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 238000009689 gas atomisation Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000005415 magnetization Effects 0.000 abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 47
- 229910052761 rare earth metal Inorganic materials 0.000 description 18
- 150000002910 rare earth metals Chemical class 0.000 description 17
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000345998 Calamus manan Species 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- LFYJSSARVMHQJB-QIXNEVBVSA-N bakuchiol Chemical compound CC(C)=CCC[C@@](C)(C=C)\C=C\C1=CC=C(O)C=C1 LFYJSSARVMHQJB-QIXNEVBVSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
Abstract
The invention provides the preparation method of a kind of permanent-magnet material and permanent-magnet material, to improve the saturation magnetization and high-coercive force of permanent-magnet material.Wherein, the main component of the permanent-magnet material is SmxFe(1‑x‑y)My, wherein M is selected from any of Ti, V, Mo and Co or a variety of, and x scope is 40~50wt%, and y scope is 0~5wt%；The crystal grain of permanent-magnet material is anisotropic flaky crystalline grain, and the size of the width of flaky crystalline grain is 20~80nm, and the size of the length direction of flaky crystalline grain is 50~300nm.Because the crystal grain of the permanent-magnet material is anisotropic flaky crystalline grain, so as to improve the saturation magnetization of the permanent-magnet material.Simultaneously as the size of the width of the flaky crystalline grain is 20~80nm, the size of the length direction of flaky crystalline grain is 50~300nm, so as to improve the coercivity of permanent-magnet material.
Description
Technical field
The present invention relates to permanent-magnet material technical field, in particular to the preparation of a kind of permanent-magnet material and permanent-magnet material
Method.
Background technology
In recent years, the Trend of Permanent using rare earth permanent-magnetic material as representative is very fast.Found from 1960s
Since first generation rare earth permanent-magnetic material, SmCo is successively developed5、Sm2Co17And Nd2Fe14Three generations's rare-earth permanent magnet such as B,
And the maximum magnetic energy product of rare-earth permanent magnet performance is represented from 20MGOe liftings to 59.6MGOe.The technique for preparing rare-earth permanent magnet
Generally include prior powder metallurgy technique for preparing sintered rare-earth permanent magnetic body and for preparing binding rare earth permanent magnet
M elt-spun overqu- enching.Wherein, the rare-earth permanent magnet prepared by prior powder metallurgy technique has excellent magnetic property and close
The magnet structure of theoretical density, makes it be obtained a wide range of applications in magneto field；And m elt-spun overqu- enching with its it is near eventually into
The characteristic of type also obtains important application.
At present, the research of rare earth permanent-magnetic material is concentrated mainly on new material system and new preparation method aspect.Wherein,
Metastable state Sm systems rare earth permanent magnet causes the research interest of people, this be primarily due to its have high intrinsic magnetic property and
Complicated structure transformation, makes people constantly be optimized in terms of structure, composition, microstructure to it.For example, Katter etc.
People uses the technique study of magnetron sputtering Sm5(Fe, Ti)17Compound, it is found that it has high-coercive force.Shenyang metal is used
The technique study of mechanical alloying SmFeTi serial rare-earth permanent-magnet materials.The neat rattan wise man of Chiba, Japan polytechnical university, which controls et al., to adopt
Sm is have studied with quick-quenching method5Fe17Compound, it is found that its coercivity can be up to 35kOe.
For Sm5Fe17For permanent-magnet material, Sm is mainly used to provide high anisotropy field, so that permanent-magnet material is obtained
Obtain high coercivity (i.e. Sm5Fe17The anisotropy of the crystal grain of permanent-magnet material is higher, and its coercivity is higher), and iron is mainly used to
High atomic magnetic moment is provided, makes Sm5Fe17Permanent-magnet material obtains high saturation magnetization.But, conventional preparation Sm5Fe17Forever
The method of magnetic material can only prepare amorphous Sm by rapid quenching5Fe17Permanent-magnet powder, then to amorphous Sm5Fe17Forever
Magnetic powder is heat-treated (sintering) to prepare magnetic, then prepares bulk by way of being bonded with binding agent
Sm5Fe17Permanent-magnet material.
However, due to Sm5Fe17Fe contents are less in permanent-magnet material, cause Sm5Fe17The saturation magnetization of permanent-magnet material
It is low.Meanwhile, Sm5Fe17The principal crystalline phase of permanent-magnet material is metastable Sm5Fe17Phase, the Sm5Fe17Easily occur to divide under phase high temperature
Solution, therefore, it is difficult to fine and close sintered magnet is prepared by traditional sintering process.And what traditional quick-quenching method was prepared from
The crystal grain of Sm5Fe17 permanent-magnet materials is in isotropism (i.e. crystal grain No yield point), so that formed Sm5Fe17The magnetic of permanent-magnet material
Square orientation is relatively disperseed, and ultimately results in Sm5Fe17The coercivity of permanent-magnet material is relatively low.
The content of the invention
It is a primary object of the present invention to provide the preparation method of a kind of permanent-magnet material and permanent-magnet material, to improve permanent magnetism material
The saturation magnetization and coercivity of material.
To achieve these goals, according to an aspect of the invention, there is provided a kind of permanent-magnet material, the permanent-magnet material
Main component is SmxFe(1-x-y)My, wherein M is selected from any of Ti, V, Mo and Co or a variety of, x scope for 40~
50wt%, y scope are 0~5wt%；The crystal grain of permanent-magnet material is anisotropic flaky crystalline grain, and the width of flaky crystalline grain
The size in direction is 20~80nm, and the size of the length direction of flaky crystalline grain is 50~300nm.
Further, the ratio between the size of the length direction of flaky crystalline grain and the size of width of flaky crystalline grain ＞ 2.
Further, the length direction of flaky crystalline grain and easy axis direction are same or like.
Further, the size of the width of flaky crystalline grain is 20~60nm, the size of the length direction of flaky crystalline grain
For 50~200nm；Y scope is 0~3wt%.
Further, the principal crystalline phase of permanent-magnet material is Sm5Fe17, the secondary crystalline phase of permanent-magnet material includes SmFe2And/or SmFe3。
Further, mass percent≤5% of the secondary crystalline phase of permanent-magnet material.
According to another aspect of the present invention there is provided a kind of preparation method of permanent-magnet material, the preparation method includes following
Step：Amorphous permanent-magnet powder is prepared, the main component of amorphous permanent-magnet powder is SmxFe(1-x-y)My, wherein M choosings
From any of Ti, V, Mo and Co or a variety of, x scope is 40~50wt%, and y scope is 0~5wt%；To amorphous state
Permanent-magnet powder carry out being heat-treated to the permanent-magnet powder to form crystalline state；And hot compression deformation processing is carried out to the permanent-magnet powder of crystalline state
Size to permanent-magnet material of the formation with anisotropic flaky crystalline grain, and the width of flaky crystalline grain is 20~80nm,
The size of the length direction of flaky crystalline grain is 50~300nm.
Further, in the step of forming the permanent-magnet powder of crystalline state, amorphous permanent-magnet powder is carried out to be heat-treated to shape
It is Sm into principal crystalline phase5Fe17Crystalline state permanent-magnet powder.
Further, the temperature of heat treatment is 600~900 DEG C, and the time of heat treatment is 2~30h.
Further, the step of hot compression deformation is handled includes：The permanent-magnet powder of crystalline state is carried out at first time hot compression deformation
Reason has the blank of isotropic crystal grain to being formed；And blank is carried out second of hot compression deformation processing to form permanent magnetism material
Material.
Further, the step of first time hot compression deformation is handled includes：The permanent-magnet powder of crystalline state is put into hot-press equipment,
And in a vacuum or inert atmosphere to the pressure that application pressure is 100~300MPa on the permanent-magnet powder of crystalline state；At the uniform velocity it is warming up to
It is incubated after 600~800 DEG C；Release, which is cooled to after normal temperature and pressure, obtains blank.
Further, the step of second of hot compression deformation is handled includes：Blank is put into hot-press equipment, and 600~
It is incubated at a temperature of 800 DEG C；Gradually pressure is applied pressure to blank reach 100~300MPa；Release is cooled to normal temperature
Permanent-magnet material is obtained after normal pressure.
Further, the technique of the processing of first time hot compression deformation and second of hot compression deformation processing is discharge plasma sintering
Or electric heating sintering.
Further, temperature of the temperature less than heat treatment of hot compression deformation processing.
Further, the temperature of hot compression deformation processing is lower than the temperature of heat treatment more than 50 DEG C.
Further, the method for preparing amorphous phase permanent-magnet powder is rapid quenching or gas atomization.
Apply the technical scheme of the present invention, be Sm the invention provides a kind of main componentxFe(1-x-y)MyPermanent-magnet material,
Wherein M is selected from any of Ti, V, Mo and Co or a variety of, and x scope is 40~50wt%, and y scope is 0~5wt%, forever
The crystal grain of magnetic material is anisotropic flaky crystalline grain, and the size of the width of flaky crystalline grain is 20~80nm, flake crystalline
The size of the length direction of grain is 50~300nm.Due to Sm5Fe17Its higher coercivity of anisotropy of the crystal grain of permanent-magnet material
It is higher, and the crystal grain of the permanent-magnet material is anisotropic flaky crystalline grain, so that the saturated magnetization for improving the permanent-magnet material is strong
Degree, solve in permanent-magnet material due to content of rare earth is high and the problem of saturation magnetization that iron content is caused less is relatively low.Meanwhile,
Because in certain grain size range, the smaller coercivity of crystallite dimension is higher, and the chi of the width of the flaky crystalline grain
Very little is 20~80nm, and the size of the length direction of flaky crystalline grain is 50~300nm, so that the coercivity of permanent-magnet material is improved,
And then improve the overall magnetic property of permanent-magnet material.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the schematic flow sheet of the preparation method for the permanent-magnet material that embodiment of the present invention is provided.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.Describe the application in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
From background technology, the saturation magnetization and coercivity of existing permanent-magnet material are reduced.The present inventor
Studied that there is provided a kind of permanent-magnet material regarding to the issue above.The main component of the permanent-magnet material is SmxFe(1-x-y)My, its
Middle M is selected from any of Ti, V, Mo and Co or a variety of, and x scope is 40~50wt%, and y scope is 0~5wt%；Permanent magnetism
The crystal grain of material is anisotropic flaky crystalline grain, and the size of the width of flaky crystalline grain is 20~80nm, flaky crystalline grain
Length direction size be 50~300nm.
In above-mentioned permanent-magnet material, due to Sm5Fe17Its higher coercivity of anisotropy of the crystal grain of permanent-magnet material is higher, and
The crystal grain of the permanent-magnet material is anisotropic flaky crystalline grain, so as to improve the saturation magnetization of the permanent-magnet material, is solved
In permanent-magnet material due to content of rare earth is high and the problem of saturation magnetization that iron content causes less is relatively low.Simultaneously as
In certain grain size range, the smaller coercivity of crystallite dimension is higher, and the size of the width of the flaky crystalline grain is 20
~80nm, the size of the length direction of flaky crystalline grain is 50~300nm, so as to improve the coercivity of permanent-magnet material, Jin Erti
The high overall magnetic property of permanent-magnet material.
The main component of above-mentioned permanent-magnet material is SmFe bases, and a certain amount of M (M=Ti, V, Mo, Co) can be added wherein
Improve the performances such as corrosion resistance.Wherein, M is preferably Co；M content y scope is 0~5wt.%, it is further preferable that y model
Enclose for 0~3wt%, in y=0, it is SmFe binary to represent whole composition, and y content can not be more than 5wt.%, otherwise can be significantly
The magnetic property of permanent-magnet material is reduced, preferably y scope is in the range of 3wt.%.And Sm content x scopes 40~50wt.% it
Between, the scope ensure that the principal crystalline phase of permanent-magnet material is Sm5Fe17Phase, and the scope is left, occur in material more
SmFe2、SmFe3Grade crystalline phase, so as to cause the performance of permanent-magnet material to deteriorate.By modifying ingredients and preparation technology, make secondary
Crystalline phase ratio is within 5wt.%, so as to ensure that permanent-magnet material has high magnetic characteristics.It should be noted that Rare Earth Elements of the present invention
Element is mainly Sm, but unavoidably containing rare earth impurities such as Pr, Nd, and require that the content of rare earth impurities is less than 1wt.%.
In the permanent-magnet material that provides of the present invention, it is desirable to which the crystal grain of permanent-magnet material is anisotropic flaky crystalline grain, and piece
The size of the width of shape crystal grain is 20~80nm, and the size of the length direction of flaky crystalline grain is 50~300nm.Because
Sm5Fe17Its higher coercivity of anisotropy of the crystal grain of permanent-magnet material is higher, and the crystal grain of the permanent-magnet material is anisotropic
Flaky crystalline grain, so as to improve the saturation magnetization of the permanent-magnet material, is solved in permanent-magnet material due to content of rare earth height
The problem of saturation magnetization that iron content is caused less is relatively low.Simultaneously as in certain grain size range, crystallite dimension
Smaller coercivity is higher, and the size of the width of the flaky crystalline grain is 20~80nm, the chi of the length direction of flaky crystalline grain
Very little is 50~300nm, so as to improve the coercivity of permanent-magnet material, and then improves the overall magnetic property of permanent-magnet material.More
Preferably, the size of the width of flaky crystalline grain is 20~60nm, the size of the length direction of flaky crystalline grain for 50~
200nm。
It is preferred that the size and the ratio between the size of the width ＞ of flaky crystalline grain of the length direction of flaky crystalline grain
2.The ratio between the size of the width of flaky crystalline grain and the size of length direction of flaky crystalline grain are bigger, are more conducive to improving permanent magnetism
The saturation magnetization of material.Further, the length direction of flaky crystalline grain and easy axis direction are same or like.This
When, whole permanent-magnet material is in magnetic history, and magnetic moment orientation is uniform, greatly improves its magnetic property.
According to another aspect of the present invention there is provided a kind of preparation method of permanent-magnet material, the preparation method includes following
Step：Amorphous permanent-magnet powder is prepared, the main component of amorphous phase permanent-magnet powder is SmxFe(1-x-y)My, wherein M is selected from
Any of Ti, V, Mo and Co or a variety of, x scope is 40~50wt%, and y scope is 0~5wt%；To amorphous
Permanent-magnet powder be heat-treated to the permanent-magnet powder to form crystalline state；And the permanent-magnet powder of crystalline state is carried out hot compression deformation handle to
The permanent-magnet material with anisotropic flaky crystalline grain is formed, and the size of the width of flaky crystalline grain is 20~80nm, piece
The size of the length direction of shape crystal grain is 50~300nm.
The illustrative embodiments of the preparation method of the permanent-magnet material provided according to the present invention are provided.
However, these illustrative embodiments can be implemented by many different forms, and it should not be construed to be limited solely to this
In the embodiment that is illustrated.It should be appreciated that these embodiments are provided so that disclosure herein thoroughly and
Completely, and by the design of these illustrative embodiments those of ordinary skill in the art are fully conveyed to.
First, amorphous permanent-magnet powder is prepared, the main component of amorphous phase permanent-magnet powder is SmxFe(1-x-y)My,
Wherein M is selected from any of Ti, V, Mo and Co or a variety of, and x scope is 40~50wt%, and y scope is 0~5wt%.System
The standby method for obtaining amorphous phase permanent-magnet powder can be rapid quenching or gas atomization.Amorphous phase is prepared when using rapid quenching forever
During magnetic powder, it is preferable that comprise the following steps：According to melting, fast quenching is carried out after certain composition proportion, fast quenching process is protected in Ar
Protect under atmosphere and carry out, injection pressure is 40~80kPa, molten steel is sprayed onto on the disk roller rotated with 30~80m/s, after fast quenching
Obtain amorphous permanent-magnet powder.Wherein, preferably fast quenching roller speed is in more than 30m/s, and too low fast quenching wheel speed is difficult to needed for being formed
Non crystalline structure, and be easier to SmFe occur2, SmFe3Grade crystalline phase；And with the raising of wheel speed, on the one hand can effectively obtain
Non crystalline structure, on the other hand can suppress the appearance of time crystalline phase, it is ensured that the final high-performance for obtaining permanent-magnet material.
Then, amorphous permanent-magnet powder is carried out being heat-treated to the permanent-magnet powder to form crystalline state.In the step, amorphous state
Permanent-magnet powder make principal crystalline phase Sm by certain temperature and being heat-treated to for time5Fe17Separate out.Preferably, the temperature of heat treatment
For 600~900 DEG C.If temperature is less than 600 DEG C, the effect of heat treatment is more weaker, and temperature may result in higher than 900 DEG C
The decomposition of principal crystalline phase.The time of heat treatment is to there is the Sm of complete crystalline state5Fe17Principal crystalline phase is defined, it is preferable that heat treatment time is
2~30h.It should be noted that in order to avoid Sm is oxidized, whole heat treatment process is preferably carried out in the environment of Ar protections.
Finally, hot compression deformation carried out to the permanent-magnet powder of crystalline state handle to being formed that there is anisotropic flaky crystalline grain forever
Magnetic material, and the size of the width of flaky crystalline grain is 20~80nm, the size of the length direction of flaky crystalline grain for 50~
300nm.Preferably, the step of hot compression deformation is handled includes：The permanent-magnet powder of crystalline state is carried out first time hot compression deformation handle to
Form the blank with isotropic crystal grain；And blank is carried out second of hot compression deformation processing to form permanent-magnet material.
Wherein, the step of first time hot compression deformation is handled be preferably：The permanent-magnet powder of crystalline state is put into hot-press equipment, and
In a vacuum or inert atmosphere to the pressure that application pressure is 100~300MPa on the permanent-magnet powder of crystalline state；At the uniform velocity it is warming up to 600
It is incubated after~800 DEG C；Release, which is cooled to after normal temperature and pressure, obtains blank.Now, obtain blank have it is isotropic
Crystal grain.In the preparation process of the blank, it is intended merely to make the material obtain preliminary densification, therefore, does not make Sm5Fe17Change
In the case that compound structure is decomposed, the method that can also be sintered by discharge plasma sintering (SPS), electric heating is equal to prepare
Even fine and close blank.
Preferably, the step of second of hot compression deformation is handled includes：Blank is put into hot-press equipment, and 600~800
It is incubated at a temperature of DEG C；Gradually pressure is applied pressure to blank reach 100~300MPa；Release is cooled to normal temperature and pressure
After obtain permanent-magnet material.Blank at a certain temperature after the processing (i.e. second hot compression deformation processing) of more aximal deformation value,
Material grains are plastically deformed, now, the easy magnetizing axis of crystal grain also under the effect of the pressure, along the direction of parallel pressure by
Gradually rotate, ultimately form along easy magnetizing axis (c-axis) direction grow high-orientation anisotropy laminated structure it is nanocrystalline.
In the step of second of hot compression deformation is handled, a certain amount of thermal deformation field is whole complete fine and close high-performance permanent magnet
Key prepared by material, in this process, sliding deformation growth occurs for the crystal grain of material under the short time, and makes material grains
Size does not occur in the case of significantly growing up, and the crystal grain of crystal grain from former isotropism, the No yield point of material is transformed into column
Crystal grain (its major axis is more than short axle), and be distributed each along stress direction, so that whole material magnetic moment in magnetic history takes
To uniform, and the performance for forming permanent-magnet material is greatly improved.
Because the permanent-magnet powder of the crystalline state before hot compression deformation processing is to come after Overheating Treatment, therefore in order to ensure most
The performance of whole permanent-magnet material, it is preferable that the temperature of hot compression deformation processing shape process is less than the temperature of heat treatment process, hot compression deformation
Pressure in processing procedure is preferably in 100~300MPa.It is further preferable that temperature of the temperature than heat treatment of hot compression deformation processing
It is low more than 50 DEG C.Further, since material therefor is the material of rich samarium, in order to avoid the oxidation of material, whole hot compression deformation processing
Process preferably in vacuum environment or is filled with progress in the environment of Ar is protected.
The preparation method of the permanent-magnet material of the invention provided and permanent-magnet material is be provided below in conjunction with embodiment.
Embodiment s1 to s10
The composition structure for the permanent-magnet material that embodiment s1 to s10 is provided as shown in table 1, prepares the specific of the permanent-magnet material
Technological parameter is as shown in table 2.The step of preparation method of lower permanent-magnet material is detailed below：
First, according to melting, fast quenching is carried out after certain component ratio proportioning (as shown in table 1), wherein fast quenching process exists
Carried out under Ar protective atmospheres, injection pressure is 50kPa, and molten steel is sprayed onto on the disk roller rotated with 40m/s, obtained after fast quenching
Amorphous permanent-magnet powder；
Then, amorphous permanent-magnet powder is carried out being heat-treated to principal crystalline phase Sm5Fe17Separate out, so as to obtain crystalline state forever
Magnetic powder；
Next, the permanent-magnet powder of crystalline state is put into hot pressing die, hot pressing die is put into vacuum hot-pressing equipment, and
The vacuum of hot-press equipment is kept in below 1Pa, while heating system and hydraulic system are opened, and corrective action is on mould
Pressure, then at the uniform velocity heats up, at the desired temperature heat-insulation pressure keeping from room temperature, and release cools after completion, obtains blank (i.e. the
The process of hot compression deformation processing)；
Finally, blank is placed again into hot-press equipment, after being incubated under vacuo, opens hydraulic system, it is slow to apply
Pressure, makes hot pressing blank at the uniform velocity occur thermal deformation, and slow cooling obtains permanent-magnet material (i.e. second hot pressing after the completion of thermal deformation
The process of deformation process).
Comparative example d1
The main component for the permanent-magnet material that this comparative example is provided is Sm5Fe17, the wherein crystal grain of permanent-magnet material is isotropism
Crystal grain.
The preparation method for the permanent-magnet material that this comparative example is provided comprises the following steps：
First, according to melting, fast quenching is carried out after certain component ratio proportioning (as shown in table 1), wherein fast quenching process exists
Carried out under Ar protective atmospheres, injection pressure is 50kPa, and molten steel is sprayed onto on the disk roller rotated with 40m/s, obtained after fast quenching
Amorphous permanent-magnet powder；
Then, amorphous permanent-magnet powder is carried out being heat-treated to principal crystalline phase Sm5Fe17 precipitations (the technological parameter such as institute of table 1
Show), so as to obtain the permanent-magnet powder of crystalline state.
Table 1
Table 2
As can be seen from Table 1 and Table 2, the remanent magnetism of S1~S10 sample, HCJ and maximum magnetic energy product are substantially big
Preferable magnetic property is achieved in the sample of d1 sample, therefore S1~S10.For S2, the length of flaky crystalline grain
The ratio between the size in direction and the size of width of flaky crystalline grain be less than 2, hence in so that in S1~S10 S2 overall magnetic
Can be minimum.In addition, the size of the width of flaky crystalline grain is 20~60nm, the size of the length direction of flaky crystalline grain for 50~
200nm obtains more preferable magnetic property.
As can be seen from the above embodiments, the above-mentioned example of the present invention realizes following technique effect：The invention provides
A kind of main component is SmxFe(1-x-y)MyPermanent-magnet material, wherein M is selected from any of Ti, V, Mo and Co or a variety of, x's
Scope is 40~50wt%, and y scope is 0~5wt%, and the crystal grain of permanent-magnet material is anisotropic flaky crystalline grain, and sheet
The size of the width of crystal grain is 20~80nm, and the size of the length direction of flaky crystalline grain is 50~300nm.Due to Sm5Fe17
Its higher coercivity of anisotropy of the crystal grain of permanent-magnet material is higher, and the crystal grain of the permanent-magnet material is anisotropic flake crystalline
Grain, so as to improve the saturation magnetization of the permanent-magnet material, solve in permanent-magnet material due to content of rare earth is high and iron content
The problem of saturation magnetization caused less is relatively low.
The preferred embodiments of the present invention are these are only, are not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (15)
1. a kind of permanent-magnet material, it is characterised in that the main component of the permanent-magnet material is SmxFe(1-x-y)My, wherein M is selected from
Any of Ti, V, Mo and Co or a variety of, x scope is 40~50wt%, and y scope is 0~5wt%；The permanent magnetism material
The crystal grain of material is anisotropic flaky crystalline grain, and the size of the width of the flaky crystalline grain is 20~80nm, described
The size of the length direction of shape crystal grain is 50~300nm；The principal crystalline phase of the permanent-magnet material is Sm5Fe17。
2. permanent-magnet material according to claim 1, it is characterised in that the size of the length direction of the flaky crystalline grain and institute
State the ratio between size of width of flaky crystalline grain ＞ 2.
3. permanent-magnet material according to claim 1, it is characterised in that the length direction and easy magnetizing axis of the flaky crystalline grain
Direction it is identical.
4. permanent-magnet material according to claim 1, it is characterised in that the size of the width of the flaky crystalline grain is 20
~60nm, the size of the length direction of the flaky crystalline grain is 50~200nm；The scope of the y is 0~3wt%.
5. permanent-magnet material according to any one of claim 1 to 4, it is characterised in that the secondary crystalline phase of the permanent-magnet material
Including SmFe2And/or SmFe3。
6. permanent-magnet material according to claim 5, it is characterised in that the mass percent of the secondary crystalline phase of the permanent-magnet material
≤ 5%.
7. a kind of preparation method of permanent-magnet material, it is characterised in that the preparation method comprises the following steps：
Amorphous permanent-magnet powder is prepared, the main component of amorphous permanent-magnet powder is SmxFe(1-x-y)My, wherein
M is selected from any of Ti, V, Mo and Co or a variety of, and x scope is 40~50wt%, and y scope is 0~5wt%；
Amorphous permanent-magnet powder is carried out being heat-treated to the permanent-magnet powder to form crystalline state；And
The permanent-magnet powder progress hot compression deformation of the crystalline state is handled to permanent magnetism material of the formation with anisotropic flaky crystalline grain
Material, and the size of the width of the flaky crystalline grain is 20~80nm, the size of the length direction of the flaky crystalline grain is 50
~300nm；The principal crystalline phase of the permanent-magnet material is Sm5Fe17。
8. preparation method according to claim 7, it is characterised in that the temperature of the heat treatment is 600~900 DEG C, institute
The time for stating heat treatment is 2~30h.
9. preparation method according to claim 7, it is characterised in that the step of hot compression deformation is handled includes：
The permanent-magnet powder progress first time hot compression deformation of the crystalline state is handled to blank of the formation with isotropic crystal grain；
And
The blank is carried out second of hot compression deformation processing to form the permanent-magnet material.
10. preparation method according to claim 9, it is characterised in that the step of first time hot compression deformation is handled is wrapped
Include：
The permanent-magnet powder of the crystalline state is put into hot-press equipment, and in a vacuum or inert atmosphere to the permanent magnetism powder of the crystalline state
Apply the pressure that pressure is 100~300MPa on end；
It is incubated after being at the uniform velocity warming up to 600~800 DEG C；
Release, which is cooled to after normal temperature and pressure, obtains the blank.
11. preparation method according to claim 10, it is characterised in that the step of second of hot compression deformation is handled is wrapped
Include：
The blank is put into the hot-press equipment, and is incubated at a temperature of 600~800 DEG C；
Gradually pressure is applied pressure to the blank reach 100~300MPa；
Release, which is cooled to after normal temperature and pressure, obtains the permanent-magnet material.
12. preparation method according to claim 9, it is characterised in that the first time hot compression deformation processing and described the
The technique of secondary hot pressing deformation process is that discharge plasma sintering or electric heating are sintered.
13. the preparation method according to any one of claim 7 to 12, it is characterised in that the hot compression deformation processing
Temperature is less than the temperature of the heat treatment.
14. preparation method according to claim 13, it is characterised in that the temperature of the hot compression deformation processing is than the heat
The temperature of processing is low more than 50 DEG C.
15. the preparation method according to any one of claim 7 to 12, it is characterised in that prepare the amorphous phase
The method of permanent-magnet powder is rapid quenching or gas atomization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410670051.5A CN105679479B (en) | 2014-11-20 | 2014-11-20 | The preparation method of permanent-magnet material and permanent-magnet material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410670051.5A CN105679479B (en) | 2014-11-20 | 2014-11-20 | The preparation method of permanent-magnet material and permanent-magnet material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105679479A CN105679479A (en) | 2016-06-15 |
| CN105679479B true CN105679479B (en) | 2017-08-25 |
Family
ID=56958032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410670051.5A Active CN105679479B (en) | 2014-11-20 | 2014-11-20 | The preparation method of permanent-magnet material and permanent-magnet material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105679479B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018101409A1 (en) * | 2016-11-30 | 2018-06-07 | Tdk株式会社 | Rare-earth sintered magnet |
| WO2018101408A1 (en) * | 2016-11-30 | 2018-06-07 | Tdk株式会社 | Permanent magnet and permanent magnet powder |
| CN108270327B (en) * | 2017-01-04 | 2021-02-26 | 中国科学院宁波材料技术与工程研究所 | A spherical shell-shaped permanent magnet and preparation method thereof |
| JP7124356B2 (en) * | 2018-03-09 | 2022-08-24 | Tdk株式会社 | rare earth permanent magnet |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1735947A (en) * | 2002-05-24 | 2006-02-15 | 代顿大学 | Nanocrystalline and nanocomposite rare earth permanent magnet materials and method of making the same |
| JP2011229218A (en) * | 2010-04-15 | 2011-11-10 | Minebea Co Ltd | Laminated magnet film needle |
-
2014
- 2014-11-20 CN CN201410670051.5A patent/CN105679479B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1735947A (en) * | 2002-05-24 | 2006-02-15 | 代顿大学 | Nanocrystalline and nanocomposite rare earth permanent magnet materials and method of making the same |
| JP2011229218A (en) * | 2010-04-15 | 2011-11-10 | Minebea Co Ltd | Laminated magnet film needle |
Non-Patent Citations (1)
| Title |
|---|
| Magnetic Hardening of Sm-Fe-Mo,Sm-Fe-V and Sm-Fe-Ti Magnets;L.SCHULTZ;《Journal of Magnetism and Magnetic Materials》;19901231;第83卷;全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105679479A (en) | 2016-06-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6366666B2 (en) | Method for producing sintered Nd-Fe-B magnetic body containing no heavy rare earth element | |
| CN108364736B (en) | Neodymium-iron-boron permanent magnet material and preparation method thereof | |
| CN105469917B (en) | High temperature hybrid permanent magnet and method of forming the same | |
| JP2018157197A (en) | High thermal stability rare earth permanent magnet material, method for producing the same, and magnet including the same | |
| JP2596835B2 (en) | Rare earth anisotropic powder and rare earth anisotropic magnet | |
| JP2013191814A (en) | Permanent magnet, and motor and power generator including the same | |
| JP2009302318A (en) | RL-RH-T-Mn-B-BASED SINTERED MAGNET | |
| CN105679479B (en) | The preparation method of permanent-magnet material and permanent-magnet material | |
| CN110753978B (en) | Thermally deformable magnet and method for producing same | |
| CN112216460A (en) | Nanocrystalline NdFeB magnet and preparation method thereof | |
| CN105632673B (en) | The preparation method and permanent-magnet material of permanent-magnet material | |
| CN106298132B (en) | A kind of SmCo of thermal deformation method preparation doping PrCu alloy5The method of permanent magnet | |
| CN103258609A (en) | Anisotropism nanometer rare earth permanent magnetic material and preparation method thereof | |
| JP6049661B2 (en) | permanent magnet | |
| JP6049662B2 (en) | Motors or generators, and cars | |
| CN108335900B (en) | Preparation of SmCo7Method for manufacturing/Co composite permanent magnet and magnet thereof | |
| JPH0320048B2 (en) | ||
| JPH04143221A (en) | Permanent magnet manufacturing method | |
| Lv et al. | Recent Development of Hot-Pressed-/Deformed Nd–Fe–B Permanent Magnets | |
| JPH044385B2 (en) | ||
| JPS63286515A (en) | Permanent magnet manufacturing method | |
| JPH01171207A (en) | Permanent magnet manufacturing method | |
| JPH03198302A (en) | Permanent magnet | |
| CN119008210A (en) | Method for producing RFeB-based magnet and alloy for grain boundary diffusion process used in the method | |
| CN118507190A (en) | A sintered Re-Fe-B permanent magnet and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |