CN106555041A - A kind of method of raising FeGa alloy magnetostriction performances - Google Patents
A kind of method of raising FeGa alloy magnetostriction performances Download PDFInfo
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- CN106555041A CN106555041A CN201611078322.3A CN201611078322A CN106555041A CN 106555041 A CN106555041 A CN 106555041A CN 201611078322 A CN201611078322 A CN 201611078322A CN 106555041 A CN106555041 A CN 106555041A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D6/04—Hardening by cooling below 0 degrees Celsius
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Abstract
The invention discloses a kind of method of raising FeGa alloy magnetostriction performances, belongs to field of magnetic material.The method is first put into FeGa alloy pigs in quartz ampoule, is evacuated to vacuum less than or equal to 2.5 × 10‑3Pa, is filled with protective gas；Quartz ampoule is placed in after 12～24h being incubated at 800～1000 DEG C and takes out quartz ampoule, exist side by side and carry out Quenching Treatment in sodium chloride solution；Again the FeGa alloy pigs after quenching are immersed in liquid nitrogen, subzero treatment 1～3 minute, take out FeGa alloy pigs and its temperature is warmed to room temperature；Repeat subzero treatment and temperature-rise period 0～50 time, obtain FeGa polycrystalline magnetostriction alloy materials, complete the method that the present invention improves FeGa alloy magnetostriction performances.The FeGa polycrystalline magnetostriction alloy materials obtained after the method process have big magnetostriction performance, low driving field and higher force performance.
Description
Technical field
The present invention relates to a kind of method of raising FeGa alloy magnetostriction performances, belongs to field of magnetic material.
Background technology
FeGa alloys be it is newly developed in recent years go out non-Rare-Earth Giant Magnetostrictive Materials, relative to traditional rare-earth magnetic material
Material, the material have low magnetic hysteresis, low saturation magnetic field, high magnetic intensity, excellent mechanical property and machinability, have significantly
Low-cost advantage, but its Magnetostriction also has certain gap, system with the Magnetostriction of rare earth material such as terbium dysprosium ferrum
About application of the FeGa alloys in Practical Project field, in FeGa polycrystalline material preparation technologies, majority is in heat treatment at present
Afterwards, using rolling, the complex processing method such as directional solidification makes the tissue of FeGa polycrystalline materials have preferred orientation and carry
High-magnetostriction coefficient, and emerging simple and direct technique processing method is to prepare having for high-performance big magnetostriction FeGa polycrystalline materials
Effect approach and urgent needss.
With the extensive application of liquid nitrogen, subzero treatment technology expands to the non-ferrous metals such as copper aluminum and hard alloy etc. by steel
Material, subzero treatment are the process carried out to material as cooling medium with liquid nitrogen (- 196 DEG C).It has proven convenient that subzero treatment can be steady
Determine workpiece size, improve the wearability of steel, temper resistance, corrosion resistance, impact flexibility etc..The subzero treatment of some research and probes
Structural transformation mechanism, but the transformation characteristic organized during subzero treatment does not study clear yet.
So far, there is not yet the report of FeGa polycrystalline material magnetostriction materials is processed using liquid nitrogen deep.
The content of the invention
In view of this, it is an object of the invention to provide a kind of method of raising FeGa alloy magnetostriction performances, described
The FeGa polycrystalline magnetostriction alloy materials obtained after method process have big magnetostriction performance, low driving field and higher force
Learn performance.
The purpose of the present invention is realized by technical scheme below：
A kind of method of raising FeGa alloy magnetostriction performances, methods described are comprised the following steps that：
(1) FeGa alloy pigs are put in quartz ampoule, vacuum is evacuated to less than or equal to 2.5 × 10-3Pa, is filled with protection
Gas；Quartz ampoule containing FeGa alloy pigs is placed at 800～1000 DEG C to be incubated after 12～24h and is taken out, and soaked immediately
Quenching Treatment is carried out in entering sodium chloride solution, quartz ampoule is removed, is obtained Fe-ori；
The preferred argon of the protective gas；
(2) Fe-ori is immersed in liquid nitrogen, subzero treatment 1～3 minute, takes out the Fe-ori and its temperature is risen to
Room temperature；Repeat subzero treatment and temperature-rise period 0～50 time, obtain FeGa polycrystalline magnetostriction alloy materials, complete institute of the present invention
State the method for improving FeGa alloy magnetostriction performances.
Wherein, the preferred Fe of molecular formula of the FeGa alloy pigs100-xGax, x=15～19.
Beneficial effect
(1) the method for the invention simple and fast, need not be made using complex processing methods such as rolling, directional solidifications
The internal grain of tissue produces preferred orientation, only by liquid nitrogen deep process, you can further improve Magnetostriction；Compare
In as cast condition FeGa alloy pig, FeGa polycrystalline magnetostriction alloy materials have more excellent Magnetostriction, and mangneto is stretched
Contracting performance increases stable, it is only necessary to which very low additional Magnetic driving field can use；
(2) the FeGa polycrystalline magnetostriction alloy materials that the method for the invention is obtained after processing have preferable mechanical property
Can, relatively conventional rareearth magnetic material, its Service Environment requires low, and active time increases, significantly reduce material into
This.
(3) it is simple and convenient for the relatively existing rolling course of processing of the liquid nitrogen deep process of the method for the invention choosing, into
Product rate is high, environmental protection, without the need for complicated technological process and the large-scale apparatus of costliness, can be with fast and low-cost in commercial production
Middle popularization and application.
(4) the method for the invention using liquid nitrogen process after for the lifting of Magnetostriction be it is reliable and stable, no
Can decline with the change of time.
Description of the drawings
Fig. 1 is Fe in embodiment 282Ga18The EBSD figure (EBSD figures) of polycrystalline magnetostriction alloy material；
Fig. 2 is Fe in embodiment 282Ga18Polycrystalline material be respectively Fe82-ori (original), through 10 times, 20 times, 30 times
Magneto-strain figure after processing with the liquid nitrogen deep of 40 circulations；
Fig. 3 for embodiment 2 be respectively Fe82-ori (original), at 10 times, 20 times, 30 times and 40 not good liquor nitrogen cycles
The Fe of reason82Ga18The magneto-strain figure that polycrystalline material is retested after standing one week；
Fig. 4 is Fe in embodiment 485Ga15Polycrystalline material be respectively Fe82-ori (original), through 10 times, 20 times, 30 times
With the magneto-strain figure after 40 liquid nitrogen subzero treatments；
Fig. 5 be embodiment 4 in be respectively Fe82-ori (original), through 10 times, 20 times, 30 times and 40 not good liquor nitrogen cycles
The Fe of process85Ga15Polycrystalline material standing magneto-strain figure after a week.
Specific embodiment
Below in conjunction with the accompanying drawings with specific embodiment describing the present invention, but not limited to this in detail.
The main agents information mentioned in following examples is shown in Table 1；Key instrument is shown in Table 2 with facility information.
Table 1
Table 2
The test of the magnetostriction coefficient of the magnetostriction alloy materials of FeGa polycrystalline described in following examples is using strain
Sheet resistance measurement method, it is specific as follows：
(1) direction and the crystal face of determination are chosen, and the test surfaces of all samples is identical with direction, resistance should in stickup
Become piece；
(2) sample and deformeter are connected into into a current loop, is positioned over electric magnet middle section, then Gaussmeter is pacified
It is mounted in above sample surfaces at 1mm, magnetic field is set from 0Oe to 5000Oe, from 5000Oe to -5000Oe, from -5000Oe to 0Oe,
Connection power supply proceeds by test；
(3) during changes of magnetic field, block sample length changes and causes the change of resistance-strain leaf length, enters
And causing the resistance of foil gauge to change, strain-ga(u)ge measurement obtains the change for straining sheet resistance, changing through computer software
Calculation obtains the deformation quantity of sample, the i.e. size of magnetostrictive strain value.
Embodiment 1
A kind of as cast condition Fe82Ga18The preparation method of alloy pig, methods described are comprised the following steps that：
(1) dispensing
Polished as raw material, first its surface oxidation with pure gallium of pure iron and purity of the purity more than 99.99% more than 99.99%
Skin, then put it in the beaker containing acetone soln, beaker is put into into vibrations cleaning 5 minutes in ultrasonic washing unit, then
Be placed on filter paper with hair-dryer dry, using electronic balance according to the amount of pure iron and the material of pure gallium ratio be 82:18
Weigh 4 parts of alloy pig raw materials, every part of 30g；
(2) melting
Copper earthenware is arranged in upper in lower pure iron according to pure gallium to 4 parts of alloy pig raw materials using fine vacuum arc-melting furnace
In crucible, melting process is carried out, obtain alloy button ingot；
The melting is processed and is specially：5 × 10 are evacuated to vacuum arc melting furnace first-3Below Pa, fills 40kPa argon
After prepurging, then suction is to 5 × 10-3Below Pa；Be then charged with argon and -0.04 atmospheric pressure reached to air pressure in stove, molten
Melt back is carried out under refining electric current 2A to 4A to the alloy pig raw material, congruent melting is refined 4 times, the time of each melting is 5min, and
Electromagnetic agitation is opened in the 2nd time and the 3rd melting；
Wherein, the volume fraction purity of the argon is 99.99%；
(3) cast
Alloy button ingot is put in the hanging copper crucible of vacuum turnover panel casting furnace, under copper crucible put 5cm × 5cm ×
5mm plate copper moulds, are evacuated to 2.5 × 10 to vacuum turnover panel casting furnace-3Below Pa, first using plasma-arc by alloy knob
Button ingot is smelted into simple metal liquid, after alloy button ingot is completely melt, overturns copper crucible immediately, simple metal liquid is poured into following
In plate copper mould, simple metal liquid cooled and solidified is treated, the block sample of 2mm × 4mm × 8mm is therefrom cut out with Wire EDM
Product, are polishing to smooth, obtain as cast condition Fe82Ga18Alloy pig；
Embodiment 2
It is a kind of to improve Fe82Ga18The method of alloy magnetostriction performance, methods described comprise the steps：
(1) as cast condition Fe that will be prepared in embodiment 182Ga18Alloy pig is put in quartz ampoule, is evacuated to vacuum and is less than
2.5×10-3Pa, the argon being filled with form protective atmosphere；Box resistance heat-treatment furnace is warming up to into 800 DEG C first, 10 minutes are incubated,
Again quartz ampoule is put in box resistance heat-treatment furnace, quartz ampoule is taken out after insulation 24h, existing side by side sodium chloride solution of be dipped in
In carry out being quenched to room temperature, remove quartz ampoule, obtain Fe82-ori；
(2) Fe82-ori is immersed in liquid nitrogen, subzero treatment 1 minute, takes out the Fe82-ori and immediately using blowing
Its temperature is warmed to room temperature by blower fan；Repeat subzero treatment and temperature-rise period 10 times, 20 times, 30 times and 40 times, obtain a series of
FeGa polycrystalline magnetostriction alloy material Fe82- (i+1), completes FeGa alloy magnetostriction performances are improved described in the present embodiment
Method；
Wherein, the i represents the number of times of repetition subzero treatment and temperature-rise period.
By Fe82-ori, after just completing to stand one week under the Fe82- (i+1) after liquid nitrogen deep is processed and heated up and room temperature
Fe82- (i+1) stick foil gauge, be placed under the magnetic field of -0.5-0.5T and test its magnetostrictive strain value；As shown in Figure 2,
Compared to Fe82-ori, the magnetostrictive strain value of Fe82- (i+1) has significant raising, and highest is risen to by 87ppm
119ppm；After one week is stood under Fe82- (i+1) room temperature for repeating subzero treatment 40 times with just complete liquid nitrogen deep and process and heat up
The magnetostrictive strain value essentially identical (as shown in Figure 3) of Fe82- (i+1) afterwards, illustrates that the present embodiment methods described is processed
Rear FeGa polycrystalline magnetostriction alloy materials Magnetostriction improve with higher stability.
It is in order to verify that liquid nitrogen deep processes the mechanism for improving FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients, right
The Fe82-ori carries out EBSD tests, and test result is as shown in Figure 1, it is known that, the inside of Fe82-ori alloy materials does not have crystalline substance
The preferred orientation of grain, i.e., exist without texture, from common knowledge, can not make in alloy material only by the change of temperature
Portion's crystal grain produces the inside of the FeGa polycrystalline magnetostriction alloy materials after preferred orientation, i.e. liquid nitrogen deep are processed does not have crystal grain
Preferred orientation, illustrate liquid nitrogen deep process improve FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients mechanism with it is existing
Make the internal grain of tissue produce preferred orientation using complex processing methods such as rolling, directional solidifications in technology, enter
And the mechanism of raising magnetostriction coefficient is different, the present embodiment methods described is simply simple and direct.
Embodiment 3
It is a kind of to improve as cast condition Fe85Ga15The preparation method of alloy pig, methods described are comprised the following steps that：
(1) dispensing
Polished as raw material, first its surface oxidation with pure gallium of pure iron and purity of the purity more than 99.99% more than 99.99%
Skin, then put it in the beaker containing acetone soln, beaker is put into into vibrations cleaning 5 minutes in ultrasonic washing unit, then
Be placed on filter paper with hair-dryer dry, using electronic balance according to the amount of pure iron and the material of pure gallium ratio be 85:15
Weigh 4 parts of alloy pig raw materials, every part of 30g；
(2) melting
Copper earthenware is arranged in upper in lower pure iron according to pure gallium to 4 parts of alloy pig raw materials using fine vacuum arc-melting furnace
In crucible, melting process is carried out, obtain alloy button ingot；
The melting is processed and is specially：5 × 10 are evacuated to vacuum arc melting furnace first-3Below Pa, fills 40kPa argon
After prepurging, then suction is to 5 × 10-3Below Pa；Be then charged with argon and -0.04 atmospheric pressure reached to air pressure in stove, molten
Melt back is carried out under refining electric current 2A to 4A to the alloy pig raw material, congruent melting is refined 4 times, the time of each melting is 5min, and
Electromagnetic agitation is opened in the 2nd time and the 3rd melting；
Wherein, the volume fraction purity of the argon is 99.99%；
(3) cast
It is put into out in round-meshed quartz ampoule after the alloy button ingot prepared in step (2) is pounded frustillatum, and
The quartz ampoule is arranged in vacuum induction melting spray to cast stove, on quartz ampoule, the circle of a diameter of 6mm is placed in the underface of circular hole
Bar copper mould, to vacuum induction melting spray to cast stove evacuation to 5 × 10-3Below Pa, first use feeling answer coil-induced heating close
Golden button ingot is smelted into simple metal liquid, after alloy button ingot is completely melt, presses spray to cast valve button immediately, will be pure with air pressure
Molten metal is sprayed onto in the pole copper mould, is treated simple metal liquid cooled and solidified, is therefrom cut out 2mm × 4mm with Wire EDM
The bulk sample of × 8mm, is polishing to smooth, obtains as cast condition Fe85Ga15Alloy pig；
Wherein, the aperture of the quartz ampoule circular hole is 2mm.
Embodiment 4
It is a kind of to improve Fe85Ga15The method of alloy magnetostriction performance, methods described are comprised the following steps that：
(1) as cast condition Fe that will be prepared in embodiment 385Ga15Alloy pig is put in quartz ampoule, is evacuated to vacuum and is less than
2.5×10-3Pa, the argon being filled with form protective atmosphere；Box resistance heat-treatment furnace is warming up to into 1000 DEG C first, 10 points are incubated
Clock, then quartz ampoule is put in box resistance heat-treatment furnace, quartz ampoule is taken out after insulation 12h, existing side by side Sodium Chloride of be dipped in
Carry out being quenched to room temperature in solution, obtain Fe85-ori；
(2) Fe85-ori is immersed in liquid nitrogen, subzero treatment 1 minute, takes out the Fe85-ori and immediately using blowing
Its temperature is warmed to room temperature by blower fan；Repeat subzero treatment and temperature-rise period 10 times, 20 times, 30 times and 40 times, obtain a series of
FeGa polycrystalline magnetostriction alloy material Fe85- (i+1), completes FeGa alloy magnetostriction performances are improved described in the present embodiment
Method；
Wherein, the i represents the number of times of repetition subzero treatment and temperature-rise period.
By Fe85-ori, after just completing to stand one week under the Fe85- (i+1) after liquid nitrogen deep is processed and heated up and room temperature
Fe85- (i+1) stick foil gauge, be placed under the magnetic field of -0.5-0.5T and test its magnetostrictive strain value；As shown in Figure 4,
By Fe85- (i+1) Jing after the liquid nitrogen deep of different number of times is processed, understand with the magnetostriction change curve of changes of magnetic field, phase
Compared with Fe85-ori, the magnetostrictive strain value of Fe85- (i+1) has significant raising, and highest is risen to by 54ppm
67ppm；After one week is stood under Fe85- (i+1) room temperature for repeating subzero treatment 40 times with just complete liquid nitrogen deep and process and heat up
The magnetostrictive strain value essentially identical (as shown in Figure 5) of Fe85- (i+1) afterwards, illustrates that the present embodiment methods described is processed
Rear FeGa polycrystalline magnetostriction alloy materials Magnetostriction improve with higher stability.
It is in order to verify that liquid nitrogen deep processes the mechanism for improving FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients, right
The Fe85-ori carries out EBSD tests, and from test result, the inside of Fe85-ori alloy materials does not have crystal grain preferentially
Orientation, i.e., exist without texture, from common knowledge, produce can not the internal grain of alloy material only by the change of temperature
The inside of the FeGa polycrystalline magnetostriction alloy materials after raw preferred orientation, i.e. liquid nitrogen deep process does not have preferentially taking for crystal grain
To in illustrating the mechanism and prior art that liquid nitrogen deep processes raising FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients
Make the internal grain of tissue produce preferred orientation using the complex processing method such as rolling, directional solidification, and then improve
The mechanism of magnetostriction coefficient is different, and the present embodiment methods described is simply simple and direct.
The present invention includes but is not limited to above example, every any equivalent carried out under the principle of spirit of the present invention
Replace or local improvement, all will be regarded as within protection scope of the present invention.
Claims (3)
1. a kind of method of raising FeGa alloy magnetostriction performances, it is characterised in that：Methods described is comprised the following steps that：
(1) FeGa alloy pigs are put in quartz ampoule, vacuum is evacuated to less than or equal to 2.5 × 10-3Pa, is filled with shielding gas
Body；Quartz ampoule containing FeGa alloy pigs is placed at 800～1000 DEG C to be incubated after 12～24h and is taken out, existed side by side
Quenching Treatment is carried out in sodium chloride solution, quartz ampoule is removed, is obtained Fe-ori；
(2) Fe-ori is immersed in liquid nitrogen, subzero treatment 1～3 minute, takes out the Fe-ori and its temperature is risen to into room
Temperature；Repeat subzero treatment and temperature-rise period 0～50 time, obtain FeGa polycrystalline magnetostriction alloy materials, complete the raising
The method of FeGa alloy magnetostriction performances.
2. the method for a kind of raising FeGa alloy magnetostriction performances according to claim 1, it is characterised in that：It is described
The molecular formula of FeGa alloy pigs is Fe100-xGax, wherein, x=15～19.
3. the method for a kind of raising FeGa alloy magnetostriction performances according to claim 1, it is characterised in that：The guarantor
Shield gas is argon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109065702A (en) * | 2018-06-20 | 2018-12-21 | 西安交通大学 | A kind of platinum dopant iron gallium alloy magnetostriction materials and preparation method thereof |
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| CN102166538A (en) * | 2011-05-09 | 2011-08-31 | 兰州大学 | Device for providing low-temperature environment |
| CN102400034A (en) * | 2011-11-29 | 2012-04-04 | 东北大学 | FeGa magnetostriction alloy wire and preparation method thereof |
| CN104946979A (en) * | 2015-07-10 | 2015-09-30 | 北京航空航天大学 | Giant magnetostriction material doped with trace non-solid-solution large atoms to cause distortion enhancement and preparation method |
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| CN102166538A (en) * | 2011-05-09 | 2011-08-31 | 兰州大学 | Device for providing low-temperature environment |
| CN102400034A (en) * | 2011-11-29 | 2012-04-04 | 东北大学 | FeGa magnetostriction alloy wire and preparation method thereof |
| CN104946979A (en) * | 2015-07-10 | 2015-09-30 | 北京航空航天大学 | Giant magnetostriction material doped with trace non-solid-solution large atoms to cause distortion enhancement and preparation method |
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| 李川等: "Fe81Ga19合金晶体生长取向与磁致伸缩性能", 《物理学报》 * |
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| CN109065702A (en) * | 2018-06-20 | 2018-12-21 | 西安交通大学 | A kind of platinum dopant iron gallium alloy magnetostriction materials and preparation method thereof |
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