CN106555041B - A method of improving FeGa alloy magnetostriction performances - Google Patents
A method of improving FeGa alloy magnetostriction performances Download PDFInfo
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- CN106555041B CN106555041B CN201611078322.3A CN201611078322A CN106555041B CN 106555041 B CN106555041 B CN 106555041B CN 201611078322 A CN201611078322 A CN 201611078322A CN 106555041 B CN106555041 B CN 106555041B
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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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Abstract
The invention discloses a kind of methods improving FeGa alloy magnetostriction performances, belong to field of magnetic material.FeGa alloy pigs are first put into quartz ampoule by this method, are evacuated to vacuum degree and are less than or equal to 2.5 × 10‑3Pa is filled with protective gas；Quartz ampoule is placed at 800~1000 DEG C heat preservation 12~take out quartz ampoule afterwards for 24 hours, existing side by side to be dipped in sodium chloride solution carries out quenching treatment；Quenched FeGa alloy pigs are immersed into liquid nitrogen again, subzero treatment 1~3 minute, take out FeGa alloy pigs and are warmed to room temperature its temperature；Subzero treatment and temperature-rise period 0~50 time are repeated, FeGa polycrystalline magnetostriction alloy materials are obtained, completes the method that the present invention improves FeGa alloy magnetostriction performances.The FeGa polycrystalline magnetostriction alloy materials obtained after this method processing have big magnetostriction performance, low driving field and higher force performance.
Description
Technical field
The present invention relates to a kind of methods improving FeGa alloy magnetostriction performances, belong 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, and low saturation magnetic field, high magnetic intensity, excellent mechanical property and machinability have apparent
Low-cost advantage, but the Magnetostriction of its Magnetostriction and rare earth material such as terbium dysprosium ferrum also has certain gap, makes
About application of the FeGa alloys in Practical Project field, at present majority is to be heat-treated in FeGa polycrystalline material preparation processes
Afterwards, using rolling, the more complicated 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 active demand.
With the extensive use of liquid nitrogen, subzero treatment technology expands to the non-ferrous metals such as copper aluminium and hard alloy etc. by steel
Material, subzero treatment are the processing for using liquid nitrogen (- 196 DEG C) to be carried out as cooling medium to material.It has proven convenient that subzero treatment can be steady
Determine workpiece size, improves wearability, temper resistance, corrosion resistance, impact flexibility of steel etc..The subzero treatment of some research and probes
Structural transformation mechanism, but subzero treatment during organize transformation characteristic do not study yet it is clear.
So far, there is not yet handling the report of FeGa polycrystalline material magnetostriction materials using liquid nitrogen deep.
Invention content
In view of this, the purpose of the present invention is to provide a kind of method improving FeGa alloy magnetostriction performances, it is described
The FeGa polycrystalline magnetostriction alloy materials obtained after method processing have big magnetostriction performance, low driving field and higher force
Learn performance.
The purpose of the present invention is realized by following technical scheme：
A method of FeGa alloy magnetostriction performances being improved, the method is as follows：
(1) FeGa alloy pigs are put into quartz ampoule, are evacuated to vacuum degree and are 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 heat preservation 12~take out afterwards for 24 hours, and is soaked immediately
Enter and carry out quenching treatment in sodium chloride solution, removes quartz ampoule, obtain Fe-ori；
The preferred argon gas of protective gas；
(2) Fe-ori is immersed into liquid nitrogen, subzero treatment 1~3 minute, takes out the Fe-ori and rises to its temperature
Room temperature；Subzero treatment and temperature-rise period 0~50 time are repeated, FeGa polycrystalline magnetostriction alloy materials are obtained, completes 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.
Advantageous effect
(1) the method for the invention is simple and fast, and without rolling, the more complicated processing method such as directional solidification makes
The internal grain of tissue generates preferred orientation, is only handled by liquid nitrogen deep, you can further increase Magnetostriction；It compares
In as cast condition FeGa alloy pigs, FeGa polycrystalline magnetostriction alloy materials have more excellent Magnetostriction, and mangneto is stretched
Contracting performance, which increases, to be stablized, it is only necessary to which very low additional Magnetic driving field can be used；
(2) the FeGa polycrystalline magnetostriction alloy materials obtained after the method for the invention processing have preferable mechanical property
Can, relatively traditional rareearth magnetic material, Service Environment require it is low, active time increase, significantly reduce material at
This.
(3) liquid nitrogen deep of the method for the invention choosing is handled simple and convenient for relatively existing rolling process, at
Product rate is high, environmentally protective, can be with fast and low-cost in industrial production without complicated technological process and expensive large-scale instrument
Middle popularization and application.
(4) the method for the invention using liquid nitrogen processing after be for the promotion of Magnetostriction it is reliable and stable, no
Understand change with the time and declines.
Description of the drawings
Fig. 1 is Fe in embodiment 282Ga18The electron backscatter diffraction figure (EBSD figures) of polycrystalline magnetostriction alloy material；
Fig. 2 is Fe in embodiment 282Ga18Polycrystalline material is respectively Fe82-ori (original), by 10 times, 20 times, 30 times
Liquid nitrogen deep treated the magneto-strain figure recycled with 40 times；
Fig. 3 be embodiment 2 be respectively Fe82-ori (original), by 10 times, 20 times, 30 times and 40 not good liquor nitrogen cycles at
The Fe of reason82Ga18Polycrystalline material stands the magneto-strain figure retested after a week；
Fig. 4 is Fe in embodiment 485Ga15Polycrystalline material is respectively Fe82-ori (original), by 10 times, 20 times, 30 times
With the magneto-strain figure after 40 liquid nitrogen subzero treatments；
It is respectively Fe82-ori (original), by 10 times, 20 times, 30 times and 40 not good liquor nitrogen cycles that Fig. 5, which is in embodiment 4,
The Fe of processing85Ga15Polycrystalline material stands magneto-strain figure after a week.
Specific implementation mode
The present invention is described in detail in the following with reference to the drawings and specific embodiments, but not limited to this.
The main agents information mentioned in following embodiment 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 embodiment is using strain
Sheet resistance mensuration, it is specific as follows：
(1) determining direction and crystal face are chosen, and the test surfaces of all samples are identical with direction, resistance is answered in stickup
Become piece；
(2) sample and deformeter are connected into a current loop, is positioned over electromagnet middle section, then gaussmeter is pacified
At 1mm above sample surfaces, setting magnetic field is 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, which changes, causes the variation of resistance-strain leaf length, into
And the resistance of foil gauge is caused to change, strain-ga(u)ge measurement obtains the variation of strain sheet resistance, by changing for 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, the method are as follows：
(1) dispensing
Pure gallium using pure iron of the purity more than 99.99% with purity more than 99.99% is raw material, its surface oxidation of first polishing
Skin, then put it into the beaker containing acetone soln, beaker is put into vibrations cleaning 5 minutes in supersonic wave cleaning machine, then
Be placed on being dried with hair-dryer on filter paper, using electronic balance according to the ratio between amount of substance of pure iron and pure gallium 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 high vacuum arc-melting furnace
In crucible, melting processing is carried out, alloy button ingot is obtained；
The melting is handled：5 × 10 first are evacuated to vacuum arc melting furnace-3Pa is hereinafter, fill 40kPa argon gas
After prepurging, then suction is to 5 × 10-3Pa or less；It is then charged with air pressure in argon gas to stove and reaches -0.04 atmospheric pressure, molten
It refines and melt back is carried out to the alloy pig raw material under electric current 2A to 4A, congruent melting is refined 4 times, and 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 gas is 99.99%；
(3) it casts
Alloy button ingot is put into 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-3Pa is hereinafter, first use 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 waited for, the blocky 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
A kind of raising Fe82Ga18The method of alloy magnetostriction performance, described method includes following steps：
(1) the as cast condition Fe that will be prepared in embodiment 182Ga18Alloy pig is put into quartz ampoule, is evacuated to vacuum degree and is less than
2.5×10-3Pa, the argon gas being filled with form protective atmosphere；Box resistance heat-treatment furnace is first warming up to 800 DEG C, keeps the temperature 10 minutes,
Quartz ampoule is put into box resistance heat-treatment furnace again, quartz ampoule is taken out in heat preservation afterwards for 24 hours, exists side by side and is dipped in sodium chloride solution
In be quenched to room temperature, remove quartz ampoule, obtain Fe82-ori；
(2) Fe82-ori is immersed into liquid nitrogen, subzero treatment 1 minute, takes out the Fe82-ori and immediately using blowing
Its temperature is warmed to room temperature by wind turbine；Subzero treatment and temperature-rise period 10 times, 20 times, 30 times and 40 times are repeated, is obtained a series of
FeGa polycrystalline magnetostriction alloy material Fe82- (i+1) complete to improve FeGa alloy magnetostriction performances described in the present embodiment
Method；
Wherein, the i indicates to repeat the number of subzero treatment and temperature-rise period.
By Fe82-ori, just completes the Fe82- (i+1) after liquid nitrogen deep is handled and heated up and stand at room temperature after a week
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, highest to be risen to by 87ppm
119ppm；The Fe82- (i+1) that repetition subzero treatment is 40 times is stood at room temperature completes liquid nitrogen deep processing and heating with rigid after a week
The magnetostrictive strain value of Fe82- (i+1) afterwards is essentially identical (as shown in Figure 3), illustrates that the present embodiment the method is handled
What FeGa polycrystalline magnetostriction alloy material Magnetostrictions afterwards improved has higher stability.
It is right in order to verify the mechanism that liquid nitrogen deep processing improves FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients
The Fe82-ori carries out EBSD tests, and test results are shown in figure 1, it is known that, the inside of Fe82-ori alloy materials is without crystalline substance
The preferred orientation of grain exists without texture, by common knowledge it is found that the variation only by temperature cannot make in alloy material
Portion crystal grain generates preferred orientation, i.e. the inside of liquid nitrogen deep treated FeGa polycrystalline magnetostriction alloy materials does not have crystal grain
Preferred orientation, illustrate liquid nitrogen deep processing improve FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients mechanism with it is existing
Using rolling in technology, the more complicated processing method such as directional solidification makes the internal grain of tissue generate preferred orientation, into
And the mechanism for improving magnetostriction coefficient is different, the present embodiment the method is simply simple and direct.
Embodiment 3
A kind of raising as cast condition Fe85Ga15The preparation method of alloy pig, the method are as follows：
(1) dispensing
Pure gallium using pure iron of the purity more than 99.99% with purity more than 99.99% is raw material, its surface oxidation of first polishing
Skin, then put it into the beaker containing acetone soln, beaker is put into vibrations cleaning 5 minutes in supersonic wave cleaning machine, then
Be placed on being dried with hair-dryer on filter paper, using electronic balance according to the ratio between amount of substance of pure iron and pure gallium 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 high vacuum arc-melting furnace
In crucible, melting processing is carried out, alloy button ingot is obtained；
The melting is handled：5 × 10 first are evacuated to vacuum arc melting furnace-3Pa is hereinafter, fill 40kPa argon gas
After prepurging, then suction is to 5 × 10-3Pa or less；It is then charged with air pressure in argon gas to stove and reaches -0.04 atmospheric pressure, molten
It refines and melt back is carried out to the alloy pig raw material under electric current 2A to 4A, congruent melting is refined 4 times, and 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 gas is 99.99%；
(3) it casts
It is put into out in round-meshed quartz ampoule after the alloy button ingot being prepared in step (2) is pounded frustillatum, and
The quartz ampoule is mounted in vacuum induction melting spray to cast stove, the circle of a diameter of 6mm is placed in the underface of circular hole on quartz ampoule
Bar copper mold, to vacuum induction melting spray to cast stove evacuation to 5 × 10-3Pa is hereinafter, first use feeling answers coil-induced heating that will 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, waits for simple metal liquid cooled and solidified, 2mm × 4mm is therefrom cut out 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
A kind of raising Fe85Ga15The method of alloy magnetostriction performance, the method are as follows：
(1) the as cast condition Fe that will be prepared in embodiment 385Ga15Alloy pig is put into quartz ampoule, is evacuated to vacuum degree and is less than
2.5×10-3Pa, the argon gas being filled with form protective atmosphere；Box resistance heat-treatment furnace is first warming up to 1000 DEG C, keeps the temperature 10 points
Clock, then quartz ampoule is put into box resistance heat-treatment furnace, quartz ampoule is taken out after keeping the temperature 12h, exists side by side and is dipped in sodium chloride
It carries out being quenched to room temperature in solution, obtains Fe85-ori；
(2) Fe85-ori is immersed into liquid nitrogen, subzero treatment 1 minute, takes out the Fe85-ori and immediately using blowing
Its temperature is warmed to room temperature by wind turbine；Subzero treatment and temperature-rise period 10 times, 20 times, 30 times and 40 times are repeated, is obtained a series of
FeGa polycrystalline magnetostriction alloy material Fe85- (i+1) complete to improve FeGa alloy magnetostriction performances described in the present embodiment
Method；
Wherein, the i indicates to repeat the number of subzero treatment and temperature-rise period.
By Fe85-ori, just completes the Fe85- (i+1) after liquid nitrogen deep is handled and heated up and stand at room temperature after a week
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) after the processing of the liquid nitrogen deep of different numbers, with the magnetostriction change curve of changes of magnetic field it is found that phase
Compared with Fe85-ori, the magnetostrictive strain value of Fe85- (i+1) has significant raising, highest to be risen to by 54ppm
67ppm；The Fe85- (i+1) that repetition subzero treatment is 40 times is stood at room temperature completes liquid nitrogen deep processing and heating with rigid after a week
The magnetostrictive strain value of Fe85- (i+1) afterwards is essentially identical (as shown in Figure 5), illustrates that the present embodiment the method is handled
What FeGa polycrystalline magnetostriction alloy material Magnetostrictions afterwards improved has higher stability.
It is right in order to verify the mechanism that liquid nitrogen deep processing improves FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients
The Fe85-ori carries out EBSD tests, by test result it is found that the inside of Fe85-ori alloy materials does not have crystal grain preferentially
It is orientated, i.e., exists without texture, by common knowledge it is found that the variation only by temperature cannot be such that the internal grain of alloy material produces
The inside of raw preferred orientation, i.e. liquid nitrogen deep treated FeGa polycrystalline magnetostriction alloy materials does not have preferentially taking for crystal grain
To, illustrate liquid nitrogen deep processing improve FeGa polycrystalline magnetostriction alloy material magnetostriction coefficients mechanism in the prior art
Using rolling, the more complicated processing method such as directional solidification makes the internal grain of tissue generate preferred orientation, and then improves
The mechanism of magnetostriction coefficient is different, and the present embodiment the method is simply simple and direct.
The present invention includes but not limited to above example, it is every carried out under the principle of spirit of that invention it is any equivalent
Replacement or local improvement, all will be regarded as within protection scope of the present invention.
Claims (3)
1. a kind of method improving FeGa alloy magnetostriction performances, it is characterised in that：The method is as follows：
(1) FeGa alloy pigs are put into quartz ampoule, are evacuated to vacuum degree and are less than or equal to 2.5 × 10-3Pa is filled with protection gas
Body；Quartz ampoule containing FeGa alloy pigs is placed at 800~1000 DEG C heat preservation 12~take out afterwards for 24 hours, exists side by side and is dipped in
Quenching treatment is carried out in sodium chloride solution, is removed quartz ampoule, is obtained Fe-ori；
(2) Fe-ori is immersed into liquid nitrogen, subzero treatment 1~3 minute, takes out the Fe-ori and its temperature is risen into room
Temperature；Subzero treatment and temperature-rise period 0~50 time are repeated, FeGa polycrystalline magnetostriction alloy materials is obtained, completes the raising
The method of FeGa alloy magnetostriction performances.
2. a kind of method improving 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. a kind of method improving FeGa alloy magnetostriction performances according to claim 1, it is characterised in that：The guarantor
Shield gas is argon gas.
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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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| Fe81Ga19合金晶体生长取向与磁致伸缩性能;李川等;《物理学报》;20111231;第60卷(第9期);第1-5页 * |
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