CN107622852A - A kind of preparation method of high-coercive force manganese gallium magnetic - Google Patents
A kind of preparation method of high-coercive force manganese gallium magnetic Download PDFInfo
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Abstract
A kind of preparation method of high-coercive force manganese gallium magnetic, belongs to technical field of magnetic materials.The method that high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain, obtains Mn by levitation melting techniques firstxGa alloy cast ingots, Tetragonal is obtained after 400 DEG C~650 DEG C are annealed 1~10 day, it is put into after carrying out coarse crushing sieving in the made ball grinder of stainless steel, gasoline is used as medium combination low energy ball-milling method, the manganese gallium magnetic with higher coercivity is obtained after 0~3.5h of ball milling, its microstrain is according to composition and the difference of handling process, and size is between 0.3 1.0.The manganese gallium magnetic that the present invention is prepared by the method for coarse crushing combination low energy ball milling, avoid because of the Phase-change Problems that ballmilling energy is too high and occurs, the phenomenon of stress-induced induced magnetic anisotropy and high-coercive force is observed simultaneously, realizes that magnetic hardening provides a kind of new means for manganese gallium permanent-magnet material.
Description
Technical field
The present invention relates to a kind of method that high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain, category
In technical field of magnetic materials.
Background technology
An important branch of the permanent-magnet material as magnetic material, in the today in electronic epoch, has penetrated into people's life
Every field in work, it is set to play more and more important effect.In recent years, because the increase of rare earth resources demand causes
The critical shortage of rare earth resources, price are risen sharply, and many scholars research is put into the magnetic material of non-rare earth
In, to replace the rare earth metal of costliness, to be applied in practice.Mn-Ga alloys are due to without rare earth element, Xiang Jie
The features such as structure is abundant, intrinsic magnetic properties is various is increasingly becoming the focus of field of magnetic material.On its preparation, magnetic property change and answer
It is of common occurrence with the research report of value.Research confirms that Mn atomic weight can be shown necessarily in 50-80at.% Mn-Ga alloys
Magnetic property, the target of research is also mainly within this composition range.Research shows, Mn-Ga bianry alloy magnetocrystallines
Different in nature big, spin polarizability and Curie temperature are high, while its phase structure and magnetic property can be easily by changing composition and regulation
Preparation technology regulates and controls.Above various advantages cause Mn-Ga alloys all have necessarily potential in permanent magnetism, magnetic recording etc. should
With value.Based on Mn-Ga alloy structures and performance, the research to it at present is concentrated mainly on two aspects：D022Structure
MnxGa((2<X≤3) alloy (high manganese), and close to L10The Mn of structurexGa (1≤x≤2) alloy (spiegeleisen).Reason
Show by calculating, L10The saturation magnetization Ms of-MnGa alloys is up to 116emu/g, its theoretical maximum magnetic energy product (BH)maxThen
Up to 28MGOe is suitable with cobalt-based rare earth permanent-magnetic material.Therefore, the Mn-Ga alloys of tetragonal are considered to have in permanent magnetism
The potentiality of field application.In general, the tiny microstructure of densification, even tissue, crystal grain is to obtain high performance key.Cause
This, how by regulating and controlling microstructure, obtains Mn-Ga powder and magnet with high energy product, realizes that it is applied
It is crucial.
Although L10- MnGa theoretical magnetic energy product is up to 28MGOe, however, being to its powder or block, realizes that magnetic is hard
The means of change are all extremely limited, and the coercivity and magnetic energy product of acquisition be not also high.At present, cubic MnxThe magnetic hardening of Ga powder is only
One approach is by realizing its structure nano, i.e., reaching its crystallite dimension by the method for fast melt-quenching or high-energy ball milling
Nanoscale is simultaneously derived from coercivity.As Cui et al. [Cui, Marinescu et al.2013] passes through high-energy mechanical ball milling
Crystal grain thinning, Wenjie Gong et al. [Gong, W.J., et al. (2015)] is obtained nanocrystalline by fast quenching, is obtained respectively
With certain coercitive MnxGa powder.However, the problem of above method is difficult to overcome in the presence of some：First, using these sides
The powder of method development belongs to the manocrystalline powders of micron order size, can not obtain magnetic anisotropy, it is difficult to obtain high energy product.
Secondly, alloy phase change is easily triggered using these methods, and the crystal structure such as Mn-Ga compounds have cube, six sides, four directions, but
Only cubic D022/L10The alloy of structure just has high comprehensive magnetic energy.
For the above situation, we have invented one kind not to change cubic MnxThe basis of Ga alloy thing phases and crystallite dimension
On, by MnxMicrostrain is introduced in Ga alloy powders and directly obtains the new method of high-coercive force.We are also thus first
It is found that stress (strain) and coercivity have good corresponding relation, for congruent alloy, stress (strain) is bigger, rectifys
Stupid power is higher；Microstrain is reduced or eliminated, coercivity also decreases or even disappears (referring to accompanying drawing 1-2).
The content of the invention
For the studies above present situation, the invention provides one kind to pass through in MnxIn Ga alloy powders introduce microstrain and
High-coercive force method is directly obtained, concrete technology includes：First Mn is obtained using levitation melting techniquesxGa(1.0≤x≤3.0)
Ingot casting, then annealed processing obtain single-phase cubic MnxGa alloys.The alloy is removed into surface scale and carries out coarse crushing
Afterwards, ball-milling treatment is carried out to broken ingot casting using the method for low energy medium ball milling, acquisition has big microstrain and high-coercive force
Single-phase cubic MnxGa powder.Ball milling does not change the crystal structure and the degree of order of alloy substantially, and the influence to crystallite dimension is not yet
Greatly, but its microstrain is significantly affected, stress-induced induced magnetic anisotropy is to obtain the manganese gallium magnetic of high-coercive force
The basis of offer.
A kind of method that high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain, its specific preparation side
Method comprises the following steps：
Step 1, the metal Mn and Ga of purity more than 99% are weighed in proportion, using levitation melting techniques in indifferent gas
Body protection is lower to obtain MnxGa ingot castings, 1.0≤x≤3.0；
Step 2, the Mn that step 1 is obtainedxGa ingot castings are put into annealing furnace, are selected in vacuum or atmosphere of inert gases
Suitable annealing temperature, annealing time carry out annealing and obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after the annealing ingot casting scale removal of step 2 acquisition, using suitable ball milling electricity
Pressure, spheroid, ball-milling medium and Ball-milling Time carry out ball milling, the size of spheroid, Ball-milling Time according to sample size it is different without
Together.After appropriate ball milling, the high-coercive force manganese gallium for having a significant impact and not undergoing phase transition to microstrain can be obtained
Magnetic.
In above-mentioned steps two, according to the suitable annealing temperature of the different choice of Mn-Ga compositions and annealing time, annealing temperature
For 400~650 DEG C, annealing time is 1~10 day.
In above-mentioned steps one and step 2, melting and annealing process are carried out under vacuum or inert gas shielding, indifferent gas
Body can be argon gas or helium, preferably argon gas.
The ball milling voltage used in above-mentioned steps three is 10~60V, preferably 40~60V, further preferred 50V；Ball milling is situated between
Matter can be acetone, alcohol or aviation gasoline, preferably 120# aviation gasoline.The spheroid used can be stainless steel ball, hard
Alloying pellet, preferably stainless steel ball.According to MnxThe difference of Ga compositions should select suitable spheroid mass than w, spheroid size Φ and ball
Consume time h, the mass ratio w of spheroid：18:1≤w≤25:1, spheroid size Φ：3≤Φ≤12, therefrom optional three during ball milling
In, preferably Φ 6mm, Φ 8mm, Φ 10mm Ball-milling Times h：0 ＜ h≤3.5, for high manganese, the time phase required for ball milling
To shorter, the time of low energy alloy ball milling is relatively long.
The size of the microstrain of prepared high-coercive force manganese gallium magnetic is between 0.3-1.0 in above-mentioned steps three.
The manganese gallium magnetic that the present invention is prepared by the method for coarse crushing combination low energy ball milling, is avoided because ballmilling energy is too high
And the Phase-change Problems occurred, while the induced magnetic anisotropy of stress (strain) induction and the phenomenon of high-coercive force are observed,
Realize that magnetic hardening provides a kind of new means for manganese gallium permanent-magnet material.Due to MnxGa alloys intrinsic magnetic properties forms dependent on it
(or Mn contents), for high Mn content alloy magnetic powder, the Ball-milling Time required for obtaining big microstrain and high-coercive force is relative
It is shorter；To spiegeleisen magnetic, higher remanent magnetism is also kept while obtaining higher coercivity, makes it with more the latent of application
Power.
Brief description of the drawings
Hereinafter, embodiment of the present invention is described in detail with reference to accompanying drawing, wherein：
Fig. 1 is Mn prepared by embodiment 5-61.15Ga magnetics coercivity, microstrain with Ball-milling Time change.
Fig. 2 is Mn prepared by embodiment 5-61.15The XRD of Ga magnetic difference Ball-milling Times.
Embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1：High-coercive force Mn is prepared according to step in detail below3Ga magnetics：
Step 1,99% pure Mn and 99.5% pure Ga is completed after weighing in proportion, melting technology using smelting in suspension exists
Mn is obtained under Ar atmosphere3Ga ingot castings；
Step 2, the Mn that step 1 is obtained3Ga ingot castings carry out annealing 45min in Ar atmosphere at 500 DEG C, obtain
Obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using 50V ball milling electricity
Pressure, ratio of grinding media to material are weight than 18：1, the spheroid used is made for stainless steel, spheroid size selection Φ 6mm, Φ 8mm, Φ 10mm tri-
Kind, ball-milling medium is 120# aviation gasoline, Ball-milling Time 0.25h.Mn after ball milling3Microstrain and the coercivity difference of Ga magnetics
For 0.38,8.03kOe.
Embodiment 2：High-coercive force Mn is prepared according to step in detail below2.50Ga magnetics：
Step 1,99% pure Mn and 99.5% pure Ga is completed after weighing in proportion, melting technology using smelting in suspension exists
Mn is obtained under Ar atmosphere2.50Ga ingot castings；
Step 2, the Mn that step 1 is obtained2.50Ga ingot castings at 500 DEG C make annealing treatment 1 day in Ar atmosphere, obtain
Obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using 50V ball milling electricity
Pressure, ratio of grinding media to material are weight than 20：1, the spheroid used is made for stainless steel, spheroid size selection Φ 6mm, Φ 8mm, Φ 10mm tri-
Kind, ball-milling medium is 120# aviation gasoline, Ball-milling Time 1h, Mn after ball milling2.50Microstrain and the coercivity difference of Ga magnetics
For 0.49,7.12kOe.
Embodiment 3：High-coercive force Mn is prepared according to step in detail below1.80Ga magnetics：
Step 1,99% pure Mn and 99.9% pure Ga is completed after weighing in proportion, melting technology using smelting in suspension exists
Mn is obtained under Ar atmosphere1.80Ga ingot castings；
Step 2, the Mn that step 1 is obtained1.80Ga ingot castings at 610 DEG C make annealing treatment 7 days in Ar atmosphere, obtain
Obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using 50V ball milling electricity
Pressure, ratio of grinding media to material are weight than 21：1, the spheroid used is made for stainless steel, spheroid size selection Φ 6mm, Φ 8mm, Φ 10mm tri-
Kind, ball-milling medium is 120# aviation gasoline, Ball-milling Time 1.5h, Mn after ball milling1.80The microstrain and coercivity of Ga magnetics point
Wei 0.51,6.23kOe.
Embodiment 4：High-coercive force Mn is prepared according to step in detail below1.33Ga magnetics：
Step 1,99.5% pure Mn and 99.5% pure Ga is completed after weighing in proportion, melts technology using smelting in suspension
Mn is obtained under an ar atmosphere1.33Ga ingot castings；
Step 2, the Mn that step 1 is obtained1.33Ga ingot castings at 520 DEG C make annealing treatment 1 day in Ar atmosphere, obtain
Obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using 50V ball milling electricity
Pressure, ratio of grinding media to material are weight than 22：1, the spheroid used is made for stainless steel, spheroid size selection Φ 6mm, Φ 8mm, Φ 10mm tri-
Kind, ball-milling medium is 120# aviation gasoline, Ball-milling Time 2h, Mn after ball milling1.33Microstrain and the coercivity difference of Ga magnetics
For 0.73,5.35kOe.
Embodiment 5：High-coercive force Mn is prepared according to step in detail below1.15Ga magnetics：
Step 1,99.9% pure Mn and 99.99% pure Ga is completed after weighing in proportion, melts technology using smelting in suspension
Mn is obtained under an ar atmosphere1.15Ga ingot castings；
Step 2, the Mn that step 1 is obtained1.15Ga ingot castings at 470 DEG C make annealing treatment 2 days in Ar atmosphere, obtain
Obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using 50V ball milling electricity
Pressure, ratio of grinding media to material are weight than 25：1, the spheroid used is made for stainless steel, spheroid size selection Φ 6mm, Φ 8mm, Φ 10mm tri-
Kind, ball-milling medium is 120# aviation gasoline, Ball-milling Time 0.5h, Mn after ball milling1.15The microstrain and coercivity of Ga magnetics point
Wei 0.54,2.78kOe.
Embodiment 6：High-coercive force Mn is prepared according to step in detail below1.15Ga magnetics
Step 1,99.9% pure Mn and 99.99% pure Ga is completed after weighing in proportion, melts technology using smelting in suspension
Mn is obtained under an ar atmosphere1.15Ga ingot castings；
Step 2, the Mn that step 1 is obtained1.15Ga ingot castings at 470 DEG C make annealing treatment 2 days in Ar atmosphere, obtain
Obtain Tetragonal alloy cast ingot；
Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using 50V ball milling electricity
Pressure, ratio of grinding media to material are weight than 25：1, the spheroid used is made for stainless steel, spheroid size selection Φ 6mm, Φ 8mm, Φ 10mm tri-
Kind, ball-milling medium is 120# aviation gasoline, Ball-milling Time 3.5h, Mn after ball milling1.15The microstrain and coercivity of Ga magnetics point
Wei 0.9,4.71kOe.
Performance test
The room temperature hysteresis curve of sample is obtained using vibrating specimen magnetometer (VSM) test above example, it is obtained and rectifys
Stupid force data；Carry out that microstrain value is calculated using Jade softwares, as a result as shown in table 1.Table 1.MnxGa(1.0<x<
3.0) the room temperature coercivity and microstrain of magnetic
Claims (9)
- A kind of 1. method that high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain, it is characterised in that bag Include following steps：Step 1, after more than purity 99wt.% metal Mn and Ga are weighed in proportion, using levitation melting techniques in vacuum or Mn is obtained under inert atmospherexGa ingot castings, 1.0≤x≤3.0；Step 2, the Mn that step 1 is obtainedxGa ingot castings are put into annealing furnace, under vacuum or inert gas shielding, from suitable Annealing temperature, annealing time made annealing treatment, to obtain Tetragonal alloy cast ingot；Step 3, coarse crushing will be carried out after annealing ingot casting scale removal that step 2 obtains, using suitable ball milling voltage, ball Body, ball-milling medium and Ball-milling Time carry out ball milling, and the size of spheroid, the mass ratio of spheroid and Ball-milling Time are according to sample size It is different and different.The Tetragonal manganese gallium magnetic with big microstrain, high-coercive force is obtained by ball milling.
- 2. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that in step 2, according to the suitable annealing temperature of the different choice of Mn-Ga compositions and annealing time, annealing Temperature is 400~650 DEG C, and annealing time is 1~10 day.
- 3. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that step 1 and step 2, melting and annealing process are carried out under vacuum or inert gas shielding, inertia Gas can be argon gas or helium, preferably argon gas.
- 4. inducing the preparation method of high-coercive force manganese gallium magnetic according to a kind of microstrain described in claim 1, its feature exists In the ball milling voltage used in step 3 is 10~60V, preferably 40~60V, further preferred 50V；Ball-milling medium can be third Ketone, alcohol or aviation gasoline, preferably 120# aviation gasoline.
- 5. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that the spheroid used in step 3 can be stainless steel ball, sintered carbide ball, preferably stainless steel ball.
- 6. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that the difference according to Mn-Ga compositions should select suitable spheroid mass than w and spheroid size Φ, spheroid Mass ratio w：18:1≤w≤25:1, spheroid size Φ：3≤Φ≤12, during ball milling therefrom in optional three, preferably Φ 6mm, Φ 8mm、Φ10mm。
- 7. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that in step 3, according to MnxThe difference of Ga compositions selects different Ball-milling Times, Ball-milling Time h：0 ＜ h ≤3.5；For high manganese, the time required for mechanical milling process is relatively short, and the Ball-milling Time required for spiegeleisen is relative It is longer.
- 8. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that in step 3, according to MnxThe difference of Ga compositions and the difference of handling process, the size of its microstrain Between 0.3-1.0.
- 9. high-coercive force manganese gallium permanent-magnet powder is prepared by way of introducing microstrain according to a kind of described in claim 1 Method, it is characterised in that same substance coercivity microstrain increases and increased.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110090965A (en) * | 2019-06-10 | 2019-08-06 | 重庆理工大学 | Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder |
| CN110534328A (en) * | 2019-09-02 | 2019-12-03 | 北京工业大学 | A kind of method that liquid nitrogen cryogenics ball milling prepares high-coercive force manganese gallium magnetic powder |
| CN112195381A (en) * | 2020-10-15 | 2021-01-08 | 北京工业大学 | Preparation method of Sr-doped manganese-gallium alloy and high-coercivity nanocrystalline magnet thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110090965A (en) * | 2019-06-10 | 2019-08-06 | 重庆理工大学 | Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder |
| CN110090965B (en) * | 2019-06-10 | 2022-05-13 | 重庆理工大学 | Preparation of high coercive force superfine Sm2Co17Method for producing magnetic powder |
| CN110534328A (en) * | 2019-09-02 | 2019-12-03 | 北京工业大学 | A kind of method that liquid nitrogen cryogenics ball milling prepares high-coercive force manganese gallium magnetic powder |
| CN110534328B (en) * | 2019-09-02 | 2021-07-16 | 北京工业大学 | Method for preparing high-coercivity manganese-gallium magnetic powder through liquid nitrogen low-temperature ball milling |
| CN112195381A (en) * | 2020-10-15 | 2021-01-08 | 北京工业大学 | Preparation method of Sr-doped manganese-gallium alloy and high-coercivity nanocrystalline magnet thereof |
| WO2022077679A1 (en) * | 2020-10-15 | 2022-04-21 | 北京工业大学 | Preparation method for sr-doped manganese-gallium alloy and high coercivity nanocrystalline magnet thereof |
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