CN104947194A - Magnetostrictive material and preparation method thereof - Google Patents
Magnetostrictive material and preparation method thereof Download PDFInfo
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- CN104947194A CN104947194A CN201510221641.4A CN201510221641A CN104947194A CN 104947194 A CN104947194 A CN 104947194A CN 201510221641 A CN201510221641 A CN 201510221641A CN 104947194 A CN104947194 A CN 104947194A
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Abstract
The invention provides a magnetostrictive material and a preparation method thereof. The composition of the magnetostrictive material is (Fe[]1-x]Gax)[100-y]REy, wherein 0.17<=x<=0.19, 0.01<=y<=0.2, and RE is selected from one or more of Tb, La, Sm, Dy, Lu, Ho, Er and Tm. The preparation method comprises the following steps: smelting the Fe Ga and RE prepared according to the composition requirements into a mother alloy cast ingot, preparing a mother alloy bar, putting the mother alloy bar and a <100>-oriented FeGa monocrystal seed in a directional solidification apparatus, vacuumizing the directional solidification apparatus, charging protective gas, heating to melt all the mother alloy bar and melt the upper part of the FeGa monocrystal seed, and drawing the molten material into a coolant along the lower part of the FeGa monocrystal seed to carry out directional solidification, wherein the temperature gradient is controlled at 1*10<5>-9*10<5> K/m, and the growth rate is 1000-20000 mm/hour. The magnetostrictive material prepared by the method is a <100>-oriented monocrystal material in which the RE elements are completely dissolved in the FeGa matrix; the saturated magnetic field is only 100-5000e, and the magnetostriction coefficient is up to 300-1500 ppm; and the magnetostrictive material has favorable comprehensive usability and wide application prospects.
Description
Technical field
The present invention relates to a kind of magneticsubstance, particularly relate to a kind of magnetostriction materials and preparation method thereof.
Background technology
Magnetostriction materials are as the important ferromagnetic functional materials of a class, and its geometrical dimension can occur reversible change in all directions with the change of magnetized state, and the reversible deformation of this Magnetic Field-Induced is referred to as magnetostriction.Since joule in 1842 proposes magnetostrictive effect, magnetostriction materials are just widely applied to the numerous areas such as aviation, navigation, robot, new forms of energy, biomedicine, play an important role in national economy and industrial production.FeGa alloy as the magnetostriction materials of latest generation, the good comprehensive use properties such as low with saturation magnetic field, mechanical property good, magnetostriction is large and by extensive concern, become the strategic novel material of 21st century.
Although the comprehensive use properties of FeGa alloy is good, but traditional FeGa binary alloy saturation magnetostriction constant is only 1/5 of Terfenol-D alloy, therefore Optimization Technology prepares the monocrystal material of <100> orientation and design alloying constituent makes FeGa matrix have larger magnetostriction coefficient, becomes the inevitable choice improving further FeGa matrix Magnetostriction.At present, also mainly concentrate on raising Magnetostriction for the research of FeGa alloy and optimize on material preparation process both at home and abroad.
Publication number is that the Chinese patent of CN101086912A discloses a kind of FeGa-RE series magnetostriction material and manufacturing process thereof, and these magnetostriction materials are polycrystal.Its main component is Fe, Ga and RE, and wherein add one or more in La, Ce, Pr, Nd, Tb, Dy, content is 0.01-20at%.The manufacturing process of these magnetostriction materials comprises the alloy after by raw material refining and pours into required pole, alloy rod high-temperature gradient rapid solidification method or crystal pulling method or Bridgman method, carry out epitaxis, finally obtain the magnetostriction materials of <100> and <110> orientation.But, the magnetostriction coefficient of this material is only about 300ppm, the material Magnetostriction using this method to prepare obviously is promoted, and its reason may be that rare earth atom is pinned at grain boundaries with the precipitation of second-phase form and is not solidly soluted in FeGa matrix.
Publication number is that the Chinese patent of CN103556045A discloses one based on FeGa-RFe
2new Magnetostrictive Material of magnetocrystalline anisotropy compensation principle design and preparation method thereof, the composition of this magnetostriction polycrystalline material is (Fe
100-Xga
x)
y(RFe
2)
z, wherein 10≤X≤40, Y and Z regulates ratio Y:Z=1 ~ 20 of compensating component in pseudo-binary system, RFe
2for TbFe
2, SmFe
2, DyFe
2, HoFe
2, ErFe
2, TmFe
2in one or several.This patent by adding the rare earth elements such as Tb, Sm in FeGa alloy, and uses vacuum belt-rejecting technology to prepare the single phase homogeneous polycrystalline band of <100> orientation.But, polycrystalline beam thickness prepared by vacuum belt-rejecting technology is only tens microns, and Tape samples causes low field (< 500Oe) Magnetostriction extreme difference (< 50ppm) due to special shape anisotropy, can not meet the user demand of the magnetostrictive devices such as high-power transverter for low field high performance three-dimensional crystalline material.
Summary of the invention
The invention provides a kind of magnetostriction materials, it is the monocrystal material of <100> orientation, and material rare earth elements is solidly soluted in FeGa matrix completely, and not only magnetostriction coefficient significantly improves, in addition saturation magnetic field is relatively low, and comprehensive usability is good.
The present invention also provides a kind of preparation method of magnetostriction materials, and it is simple to operate, technique is easy to control, and can obtain Magnetostriction and the good magnetostriction materials of comprehensive usability.
The invention provides a kind of magnetostriction materials, its composition is (Fe
1-xga
x)
100-yrE
y, wherein 0.17≤x≤0.19,0.01≤y≤0.2, RE be selected from Tb, La, Sm, Dy, Lu, Ho, Er and Tm one or more.
Further, the composition of described magnetostriction materials is (Fe
0.83ga
0.17)
99.95tb
0.05, (Fe
0.83ga
0.17)
99.95sm
0.05, (Fe
0.83ga
0.17)
99.95dy
0.05, (Fe
0.83ga
0.17)
99.95ho
0.05, (Fe
0.83ga
0.17)
99.95er
0.05, (Fe
0.83ga
0.17)
99.95tm
0.05, (Fe
0.81ga
0.19)
99.95tb
0.05, (Fe
0.81ga
0.19)
99.95sm
0.05, (Fe
0.81ga
0.19)
99.95dy
0.05, (Fe
0.81ga
0.19)
99.95ho
0.05, (Fe
0.81ga
0.19)
99.95er
0.05, (Fe
0.81ga
0.19)
99.95tm
0.05, (Fe
0.83ga
0.17)
99.97lu
0.03, (Fe
0.81ga
0.19)
99.96dy
0.04, (Fe
0.82ga
0.18)
99.98sm
0.02, (Fe
0.81ga
0.19)
99.9tm
0.1, (Fe
0.81ga
0.19)
99.8la
0.2, (Fe
0.82ga
0.18)
99.8(HoEr)
0.2, (Fe
0.83ga
0.17)
99.84(SmTm)
0.16, (Fe
0.82ga
0.18)
99.85(HoErTm)
0.15or (Fe
0.81ga
0.19)
99.85(TbDyHo)
0.15.
Further, described magnetostriction materials are the monocrystal material of <100> orientation.Particularly, described magnetostriction materials are have (200) diffraction peak between 27 ° ~ 28 ° at 2 θ, and are have (400) diffraction peak between 56 ° ~ 57 ° at 2 θ; In addition, these magnetostriction materials different family of crystal planes diffraction spot quadruple is symmetrical.
Further, in described magnetostriction materials, RE is complete solid solution in FeGa matrix.The present invention does not strictly limit described complete solid solution, wherein also can comprise the situation of basic solid solution completely.Particularly, RE complete solid solution in FeGa matrix can be proved by BSE image not having or does not substantially have the pattern of RE element precipitated phase.
Further, there are many dislocation lines in described magnetostriction materials.Particularly, at least two dislocation lines in many dislocation lines are formed and intersect; Especially, many dislocation lines intersect at a place and the radial line formed from this to surrounding radiation mutually.The length of this dislocation line can be 30 ~ 150nm.
Further, the saturation magnetic field of described magnetostriction materials is 100 ~ 500Oe, such as, be 300 ~ 500Oe, is preferably 300 ~ 400Oe, more preferably 300 ~ 350Oe.
Further, the saturation magnetostriction constant of described magnetostriction materials is 300 ~ 1500ppm, is preferably 450 ~ 1500ppm, more preferably 650 ~ 1500ppm, is further preferably 1000 ~ 1500ppm.
Further, described magnetostriction materials are club-shaped material, and its diameter is 1 ~ 10mm, and length is 1 ~ 20mm, are preferably diameter 5 ~ 10mm, length 10 ~ 20mm.
The present invention also provides a kind of preparation method of above-mentioned arbitrary described magnetostriction materials, comprises the steps:
1) Fe, Ga and RE raw material is equipped with according to the component requirements of magnetostriction materials;
2) Fe, Ga and RE raw material of outfit is smelted into mother alloy ingot;
3) described mother alloy ingot is melted, and make mother alloy rod by suction pouring;
4) the FeGa single crystal seed of described mother alloy rod and <100> orientation is placed in apparatus for directional solidification; and make FeGa single crystal seed bottom immerse cooling fluid; apparatus for directional solidification to be vacuumized and after being filled with shielding gas; heating makes the complete melting of mother alloy rod and the top melting of FeGa single crystal seed; the material of melting is carried out directional freeze in the pull to cooling fluid of FeGa single crystal seed bottom, and the thermograde controlling described directional freeze is 1 × 10
5~ 9 × 10
5k/m, the speed of growth is 1000 ~ 20000mm/h, obtained described magnetostriction materials.
In the present invention, directional freeze refers to the thermograde (G) setting up specific direction in frozen metal (i.e. non-molten metal) and non-frozen metal molten mass, makes a kind of casting technique that molten mass solidifies along the direction contrary with hot-fluid; The speed of growth refers to the speed of molten mass to pull in cooling fluid.Special rare earth elements selected by the present invention has large size and large magnetocrystalline anisotropy, carries out directional freeze simultaneously and be conducive to realizing the complete solid solution of rare earth element in FeGa matrix and the single-crystal orientation of magnetostriction materials under above-mentioned specific thermograde and the speed of growth.Further, thermograde is preferably 1 × 10
5~ 5 × 10
5k/m; The speed of growth (V) is preferably 1000 ~ 10000mm/h, more preferably 2000 ~ 8000mm/h.
The present invention adopts <100> orientation FeGa single crystal seed as seed crystal when directional freeze, and becomes partially molten state when using this seed crystal; Particularly, by controlling, the mode of heating and cooling makes the melting of seed crystal top, bottom is solidified, thus make solid-liquid interface in solid-liquid phase-change process advance along seed crystal bottom when directional freeze, the advantage orientation of seed crystal is retained, thus the new crystal formed is along the lattice stacking of seed crystal, is easier to single crystal growing; In addition, by the speed of growth (more than 1000mm/h) faster, solid-liquid interface is put down by concave change, simultaneously higher thermograde (1 × 10
5more than K/m) suppress forming core, finally cause monocrystalline to be grown up, thus realize the complete solid solution of rare earth element in FeGa matrix and the <100> single-crystal orientation of magnetostriction materials.
The purity of raw material Fe, Ga and RE that the present invention selects all is greater than 99.99wt%.
In step 4 of the present invention) in, apparatus for directional solidification is vacuumized and is filled with shielding gas and comprise and implement following operation at least one times:
1.0 × 10 are evacuated to apparatus for directional solidification
-3~ 5.0 × 10
-3be filled with shielding gas after Pa, treat that the vacuum tightness in apparatus for directional solidification rises to 1.0 × 10
-1~ 5 × 10
-1inflation is stopped after Pa.
Preferably, aforesaid operations is implemented three to four times.
Further, step 4 of the present invention) in, described mother alloy rod and FeGa single crystal seed top are placed in the inside of hollow graphite heating member, heat described graphite heating body by ruhmkorff coil, to make the complete melting of mother alloy rod and the top melting of FeGa single crystal seed.
Above-mentioned type of heating, by being arranged on after graphite heating body is heated to assigned temperature by ruhmkorff coil outside graphite heating body, carrying out heat release by the thermal radiation of graphite heating body to the material be provided at its inner portion, thus realizes the heating to material.This type of heating is easy to material is heated evenly, and can realize larger temperature, less radial symmetry gradient etc., is conducive to the single-crystal orientation of material.
Further, step 4 of the present invention) in, described heating comprises implements following operation at least one times:
With the heat-up rate of 30 ~ 40 DEG C/min, graphite heating body is heated to 1550 ~ 1700 DEG C, insulation 5 ~ 15min after mother alloy rod and the top melting of FeGa single crystal seed, then with the cooling rate of 20 ~ 30 DEG C/min graphite heating body be cooled to 1450 ~ 1550 DEG C and be incubated 3 ~ 8min, then with the heat-up rate of 30 ~ 40 DEG C/min graphite heating body be heated to 1550 ~ 1700 DEG C and be incubated 5 ~ 15min.
In the present invention, the temperature of material is made to exceed its melting temperature more than 50 ~ 200 DEG C by heating, and adopt above-mentioned ad hoc fashion to carry out heating and be not only conducive to the abundant melting of material, also help passivation and the inefficacy of heterogeneous forming core in molten mass, thus the heterogeneous forming core in minimizing molten mass, and be conducive to the single-crystal orientation of material.Preferably, aforesaid operations is implemented three to four times.
In addition, step 4) in, make FeGa single crystal seed bottom immerse cooling fluid and lower end in contact water-cooled metal part, described cooling fluid is Ga-In alloy.
That is, the present invention can by heating FeGa single crystal seed top, and the mode simultaneously cooled FeGa single crystal seed bottom realizes the partially molten state of seed crystal.Particularly, when directional freeze, the mode adopting Ga-In alloy (liquid metal cooling fluid) and water-cooled metal part to combine cools, the side of Ga-In alloy to material is wherein adopted to cool, adopt the lower end of water-cooled metal part to material to cool simultaneously, which is easy to realize larger thermograde, realizes better axial cooling performance simultaneously.Water-cooled metal part refers to and adopts water to carry out the metal parts that cools as heat-eliminating medium, and not doing strict restriction to the structure of metal parts and material, such as, can be water-cooled copper fixture.
Further, step 2) comprising:
Fe, Ga and RE raw material of outfit is placed in melting equipment, 5.0 × 10 are evacuated to melting equipment
-2~ 5.0 × 10
-3be filled with shielding gas after Pa, treat that the vacuum tightness in melting equipment rises to 1.0 × 10
-1~ 5.0 × 10
-1after Pa stop inflation, implement aforesaid operations at least one times after, at melting electric current be under the condition of 100 ~ 150A melting raw material once more than, the time controlling each melting is 3 ~ 5 minutes, makes mother alloy ingot.
Preferably, melting raw material three to five times under these conditions.
Further, step 3) comprising:
Described mother alloy ingot is placed in melting equipment, 1.0 × 10 are evacuated to melting equipment
-3~ 5.0 × 10
-3be filled with shielding gas after Pa, treat that the vacuum tightness in melting equipment rises to 1.0 × 10
-1~ 5.0 × 10
-1stopping inflation after Pa, is, under the condition of 100 ~ 300A, described mother alloy ingot is fused into aluminium alloy at melting electric current, and aluminium alloy suction casting is made mother alloy rod to mould.
In concrete scheme of the present invention, described melting equipment can be the conventional equipment of this area, such as vacuum non-consumable arc-melting furnace; Described shielding gas can be the argon gas etc. of purity more than 99.99%.
Enforcement of the present invention, at least has following advantage:
1, the present invention by adding the rare earth element with large size and large magnetocrystalline anisotropy of trace in FeGa matrix, combine the directional solidification processes with higher thermograde and the speed of growth faster simultaneously, thus achieve the complete solid solution of rare earth element in FeGa matrix and the <100> single-crystal orientation of magnetostriction materials.
2, preparation method of the present invention is simple to operate, technique is easy to control, rare earth element addition is few, preparation cycle is short, particularly specific type of heating is conducive to passivation and the inefficacy of heterogeneous forming core in the abundant melting of material and molten mass, the specific type of cooling is easy to obtain larger thermograde, good cooling results, the Magnetostriction of obtained magnetostriction materials and comprehensive usability are well, applied widely.
3, the magnetostriction materials prepared by preparation method of the present invention are the monocrystal material of <100> orientation, this material rare earth elements is solidly soluted in FeGa matrix completely, saturation magnetic field is only 100 ~ 500Oe, magnetostriction coefficient is up to 300 ~ 1500ppm, comprehensive usability is good, has a extensive future.
Accompanying drawing explanation
Fig. 1 is the BSE image of mother alloy ingot prepared by the embodiment of the present invention 1;
Fig. 2 is the XRD figure spectrum of mother alloy rod prepared by the embodiment of the present invention 1;
Fig. 3 is the BSE image of magnetostriction materials prepared by the embodiment of the present invention 1;
Fig. 4 is synchrotron radiation X RD collection of illustrative plates and the Laue diffracting spectrum of magnetostriction materials prepared by the embodiment of the present invention 1.
Fig. 5 is the Fe that the embodiment of the present invention 1 adopts
83ga
17the TEM image of single crystal seed;
Fig. 6 is the TEM image of magnetostriction materials prepared by the embodiment of the present invention 1;
Fig. 7 is the Fe that the embodiment of the present invention 1 adopts
83ga
17the Magnetostrictive curve of the magnetostriction materials of single crystal seed and preparation.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with drawings and Examples of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1 prepares (Fe
0.83ga
0.17)
99.95tb
0.05
Prepared composition is (Fe
0.83ga
0.17)
99.95tb
0.05the method of magnetostriction materials, comprise the steps:
1, prepare burden
The purity of raw material Fe, Ga and Tb (RE raw material) of selecting all is greater than 99.99wt%, and in order to prevent melting loss of elements in fusion process, when being equipped with Fe, Ga and Tb raw material according to mentioned component, add Ga and Tb respectively according to the scaling loss amount of about 1wt%.Particularly, take the Tb of Ga and 0.048g of Fe, 7.158g of 27.72g, for subsequent use.
2, mother alloy ingot is prepared
Raw material Fe, Ga and RE of above-mentioned outfit are put into the crucible of vacuum non-consumable arc-melting furnace, when placing, the metallic element of easy scaling loss is placed in crucible bottom, and not easily the metallic element of scaling loss is placed in above crucible.
4.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-3after Pa, in body of heater, be filled with high-purity argon gas, the volumn concentration (purity) of argon gas is more than 99.99%, treats that the vacuum tightness in stove rises to 1.0 × 10
-1pa stops inflation later, repeatedly after this step operation three times, melting electric current is set to 150A, melting is carried out to raw material, the time controlling each melting is about 4 minutes, melt back four times, obtained mother alloy ingot, carry out electron probe test to this mother alloy ingot, its backscattered electron (BSE) image as shown in Figure 1; As can be seen from Figure 1, in the mother alloy ingot material under as cast condition, Tb element is distributed widely in FeGa matrix grain boundaries with the form of second-phase.
3, mother alloy rod is prepared
Above-mentioned obtained master alloy ingot is placed in vacuum non-consumable arc-melting furnace, 3.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-3after Pa, in body of heater, be filled with the high-purity argon gas that volumn concentration is more than 99.99%, treat that in stove, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later.
Melting electric current is set to 150A, master alloy melting ingot, when master alloy ingot soon melts rapidly by melting current setting to 300A, aim at master alloy ingot center, mould hole place arc blow-out, open suction pouring valve simultaneously, utilize negative pressure the suction of the mother alloy liquid of instant melting to be cast onto in mould and make mother alloy rod, its XRD figure spectrum as shown in Figure 2; Result shows: this mother alloy rod is polycrystalline tissue, and polycrystalline orientation is based on <110>, <100>.
4, magnetostriction materials are prepared
By above-mentioned obtained mother alloy rod outside surface grinding homogeneity, with the Fe of <100> orientation
83ga
17single crystal seed is together soaked in acetone, and ultrasonic cleaning 10min under the frequency of 50KHz, is put in after cleaning in baking oven, dries 20min in 120 DEG C, obtains washed samples.
Adopt directional solidification furnace to carry out directional freeze to material, first graphite heating body is placed on insulation ring, and insulation ring is placed on GaIn alloy tank; Secondly washed samples being put into alumina crucible, when placing, mother alloy rod being placed on Fe
83ga
17the top of single crystal seed, and top crucible being positioned over the inner center of cylindrical hollow graphite heating body and GaIn alloy tank; Again crucible is fallen in GaIn alloy tank, make the Fe in crucible
83ga
17the bottom of single crystal seed is immersed the GaIn alloy in GaIn alloy tank and makes Fe
83ga
17the contact surface of single crystal seed and mother alloy rod is positioned at the ullage of GaIn alloy; Meanwhile, arrange water-cooled copper fixture below seed crystal, and the lower end of seed crystal is formed with water-cooled copper fixture contact, water-cooled copper fixture adopts the cold water of about 5 DEG C to carry out circulating cooling.
Subsequently, 3.0 × 10 are evacuated to directional solidification furnace
-3after Pa, in body of heater, be filled with the high-purity argon gas that volumn concentration is more than 99.99%, treat that in stove, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later, repeatedly after this step operation three times, with the heat-up rate of 35 DEG C/min, graphite heating body is heated to 1600 DEG C, treats mother alloy rod melting and Fe completely
83ga
1710min is incubated after the melting of single crystal seed top, then with the cooling rate of 25 DEG C/min, the temperature of graphite heating body is down to 1500 DEG C, be incubated 5min at such a temperature, with identical heat-up rate graphite heating body be heated to 1600 DEG C again and be incubated 10min, 30min is incubated, mother alloy rod melting and Fe completely after the above operation of circulation three times
83ga
17the partially molten state that single crystal seed becomes top melting, bottom is solidified.
Control temperature gradient is 1 × 10
5k/m, the speed of growth is 20000mm/h, the material of melting is carried out directional freeze in FeGa single crystal seed lower flat quietly downward pull to GaIn alloy, during directional freeze, by GaIn alloy cooling fluid, material side is cooled, by water-cooled copper fixture, material lower end is cooled simultaneously, make single crystal growing; After growth terminates, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, obtained composition is (Fe
0.83ga
0.17)
99.95tb
0.05bar-shaped magnetostriction materials (size Φ 7mm × 20mm), its BSE image and synchrotron radiation X RD collection of illustrative plates and Laue diffracting spectrum are respectively as shown in Figure 3 and Figure 4, Fig. 3 shows do not have RE element precipitated phase in these magnetostriction materials, Fig. 4 shows that these magnetostriction materials are have (200) diffraction peak between 27 ° ~ 28 ° at 2 θ, and be, between 56 ° ~ 57 °, there is (400) diffraction peak at 2 θ, in addition, these magnetostriction materials different family of crystal planes diffraction spot quadruple is symmetrical.Illustrate thus: should (Fe
0.83ga
0.17)
99.95tb
0.05in magnetostriction materials, Tb element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation.
Respectively to Fe
83ga
17(the Fe of single crystal seed and preparation
0.83ga
0.17)
99.95tb
0.05magnetostriction materials carry out transmissioning electric mirror test, and observe the dark field image under material STEM pattern along <100> zone axis, result as shown in Figure 5 and Figure 6.Result shows: common Fe
83ga
17monocrystalline interior microscopic homogeneous microstructure consistent (Fig. 5), the and (Fe of preparation
0.83ga
0.17)
99.95tb
0.05obviously a large amount of dislocation lines can be observed in material, many dislocation line intersects at a place and the radial line formed from this to surrounding radiation mutually, and the length of dislocation line is 30 ~ 150nm, reason may be that the solid solution of Tb element causes FeGa matrix to produce tetragonal distortion, distortion causes creating internal stress in body material, and internal stress is showed by the form of dislocation line.
In addition, magnetostriction measurement system (Beijing WuKe opto-electrical Technology Co., Ltd's production) is adopted to measure (Fe
0.83ga
0.17)
99.95tb
0.05material and Fe
83ga
17the magnetostrictive strain value of monocrystalline, wherein foil gauge adopts Japanese republicanism KFG-1-120-C1-11L3M2R type resistance strain gage, and result as shown in Figure 7.Result shows: (Fe
0.83ga
0.17)
99.95tb
0.05the saturation magnetostriction constant of material is 463ppm, and it compares Fe
83ga
17the magnetostriction coefficient of monocrystalline improves about 50%; In addition, (Fe
0.83ga
0.17)
99.95tb
0.05the saturation magnetic field of material is only about 300Oe, Magnetostriction and comprehensive usability good.
Embodiment 2 prepares (Fe
0.83ga
0.17)
99.97lu
0.03
Except in batching step, the Lu taking Ga and 0.031g of Fe, 7.242g of 28.05g is for subsequent use; Prepare in magnetostriction materials step, graphite heating body is heated to 1575 DEG C, and control temperature gradient is 5 × 10
5k/m, the speed of growth is outside 8000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.83ga
0.17)
99.97lu
0.03magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.83ga
0.17)
99.97lu
0.03in magnetostriction materials, Lu element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.83ga
0.17)
99.97lu
0.03the saturation magnetostriction constant of material is 330ppm, and saturation magnetic field is about 350Oe, Magnetostriction and comprehensive usability good.
Embodiment 3 prepares (Fe
0.81ga
0.19)
99.96dy
0.04
Prepared composition is (Fe
0.81ga
0.19)
99.96dy
0.04the method of magnetostriction materials, comprise the steps:
1, prepare burden
Take the Dy of Ga and 0.04g of Fe, 8.25g of 27.88g, for subsequent use.
2, mother alloy ingot is prepared
Raw material Fe, Ga and Dy of above-mentioned outfit are put into the crucible of vacuum non-consumable arc-melting furnace, 1.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-3after Pa, in body of heater, be filled with the high-purity argon gas that purity is more than 99.99%, treat that the vacuum tightness in stove rises to 5.0 × 10
-1pa stops inflation later, and repeatedly after this step operation three times, melting electric current is set to 120A, carries out melting to raw material, the time controlling each melting is about 5 minutes, melt back four times, obtained mother alloy ingot.
3, mother alloy rod is prepared
Above-mentioned obtained master alloy ingot is placed in vacuum non-consumable arc-melting furnace, 1.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-3after Pa, in body of heater, be filled with the high-purity argon gas that purity is more than 99.99%, treat that in stove, vacuum tightness rises to 5.0 × 10
-1pa stops inflation later.
Melting electric current is set to 120A, master alloy melting ingot, when master alloy ingot soon melts rapidly by melting current setting to 300A, aim at master alloy ingot center, mould hole place arc blow-out, open suction pouring valve simultaneously, utilize negative pressure the suction of the mother alloy liquid of instant melting to be cast onto in mould and make mother alloy rod, this mother alloy rod is polycrystalline tissue, and polycrystalline orientation is based on <110>, <100>.
4, magnetostriction materials are prepared
To the Fe of above-mentioned obtained mother alloy rod and <100> orientation
81ga
19single crystal seed is cleaned, and obtains washed samples.
Adopt directional solidification furnace to carry out directional freeze to material, after placing material according to embodiment 1 method, 1.0 × 10 are evacuated to directional solidification furnace
-3pa, is filled with the high-purity argon gas that purity is more than 99.99% in body of heater, treats that in stove, vacuum tightness rises to 5.0 × 10
-1pa stops inflation later, repeatedly after this step operation three times, with the heat-up rate of 40 DEG C/min, graphite heating body is heated to 1575 DEG C, treats mother alloy rod melting and Fe completely
81ga
195min is incubated after the melting of single crystal seed top, then with the cooling rate of 30 DEG C/min, the temperature of graphite heating body is down to 1500 DEG C, be incubated 3min at such a temperature, with identical heat-up rate graphite heating body be heated to 1575 DEG C again and be incubated 5min, 30min is incubated, mother alloy rod melting and Fe completely after the above operation of circulation three times
81ga
19the partially molten state that single crystal seed becomes top melting, bottom is solidified.
Control temperature gradient is 4 × 10
5k/m, the speed of growth is 5000mm/h, the material of melting is carried out directional freeze in FeGa single crystal seed lower flat quietly downward pull to GaIn alloy, during directional freeze, by GaIn alloy cooling fluid, material side is cooled, by water-cooled copper fixture, material lower end is cooled simultaneously, make single crystal growing; After growth terminates, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, obtained composition is (Fe
0.81ga
0.19)
99.96dy
0.04magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.81ga
0.19)
99.96dy
0.04in magnetostriction materials, Dy element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.81ga
0.19)
99.96dy
0.04the saturation magnetostriction constant of material is 454ppm, and saturation magnetic field is about 300Oe, Magnetostriction and comprehensive usability good.
Embodiment 4 prepares (Fe
0.82ga
0.18)
99.98sm
0.02
Except in batching step, the Sm taking Ga and 0.019g of Fe, 7.79g of 28.12g is for subsequent use; Prepare in magnetostriction materials step, adopt Fe
82ga
18single crystal seed is as seed crystal, and control temperature gradient is 10 × 10
5k/m, the speed of growth is outside 1000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.82ga
0.18)
99.98sm
0.02magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.82ga
0.18)
99.98sm
0.02in magnetostriction materials, Sm element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.82ga
0.18)
99.98sm
0.02the saturation magnetostriction constant of material is 315ppm, and saturation magnetic field is about 400Oe, Magnetostriction and comprehensive usability good.
Embodiment 5 prepares (Fe
0.81ga
0.19)
99.9tm
0.1
Prepared composition is (Fe
0.81ga
0.19)
99.9tm
0.1the method of magnetostriction materials, comprise the steps:
1, prepare burden
Take the Tm of Ga and 0.105g of Fe, 8.21g of 27.76g, for subsequent use.
2, mother alloy ingot is prepared
Raw material Fe, Ga and Tm of above-mentioned outfit are put into the crucible of vacuum non-consumable arc-melting furnace, 5.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-2after Pa, in body of heater, be filled with the high-purity argon gas that purity is more than 99.99%, treat that the vacuum tightness in stove rises to 1.0 × 10
-1pa stops inflation later, and repeatedly after this step operation three times, melting electric current is set to 100A, carries out melting to raw material, the time controlling each melting is about 5 minutes, melt back four times, obtained mother alloy ingot.
3, mother alloy rod is prepared
Above-mentioned obtained master alloy ingot is placed in vacuum non-consumable arc-melting furnace, 5.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-2after Pa, in body of heater, be filled with the high-purity argon gas that purity is more than 99.99%, treat that in stove, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later.
Melting electric current is set to 100A, master alloy melting ingot, when master alloy ingot soon melts rapidly by melting current setting to 300A, aim at master alloy ingot center, mould hole place arc blow-out, open suction pouring valve simultaneously, utilize negative pressure the suction of the mother alloy liquid of instant melting to be cast onto in mould and make mother alloy rod, this mother alloy rod is polycrystalline tissue, and polycrystalline orientation is based on <110>, <100>.
4, magnetostriction materials are prepared
To the Fe of above-mentioned obtained mother alloy rod and <100> orientation
81ga
19single crystal seed is cleaned, and obtains washed samples.
Adopt directional solidification furnace to carry out directional freeze to material, after placing material according to embodiment 1 method, 5.0 × 10 are evacuated to directional solidification furnace
-2pa, is filled with the high-purity argon gas that purity is more than 99.99% in body of heater, treats that in stove, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later, repeatedly after this step operation three times, with the heat-up rate of 30 DEG C/min, graphite heating body is heated to 1650 DEG C, treats mother alloy rod melting and Fe completely
81ga
1915min is incubated after the melting of single crystal seed top, then with the cooling rate of 20 DEG C/min, the temperature of graphite heating body is down to 1500 DEG C, be incubated 8min at such a temperature, with identical heat-up rate graphite heating body be heated to 1650 DEG C again and be incubated 15min, 35min is incubated, mother alloy rod melting and Fe completely after the above operation of circulation three times
81ga
19the partially molten state that single crystal seed becomes top melting, bottom is solidified.
Control temperature gradient is 5 × 10
5k/m, the speed of growth is 6000mm/h, the material of melting is carried out directional freeze in FeGa single crystal seed lower flat quietly downward pull to GaIn alloy, during directional freeze, by GaIn alloy cooling fluid, material side is cooled, by water-cooled copper fixture, material lower end is cooled simultaneously, make single crystal growing; After growth terminates, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, obtained composition is (Fe
0.81ga
0.19)
99.9tm
0.1magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.81ga
0.19)
99.9tm
0.1in magnetostriction materials, Tm element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.81ga
0.19)
99.9tm
0.1the saturation magnetostriction constant of material is 667ppm, and saturation magnetic field is about 370Oe, Magnetostriction and comprehensive usability good.
Embodiment 6 prepares (Fe
0.81ga
0.19)
99.8la
0.2
Except in batching step, the La taking Ga, 0.086g of Fe, 8.15g of 27.55g is for subsequent use; Prepare in magnetostriction materials step, adopt Fe
81ga
19graphite heating body as seed crystal, and is heated to 1650 DEG C by single crystal seed, and control temperature gradient is 8 × 10 in addition
5k/m, the speed of growth is outside 7000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.81ga
0.19)
99.8la
0.2magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.81ga
0.19)
99.8la
0.2in magnetostriction materials, La element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.81ga
0.19)
99.8la
0.2the saturation magnetostriction constant of material is 1316ppm, and saturation magnetic field is about 500Oe, Magnetostriction and comprehensive usability good.
Embodiment 7 prepares (Fe
0.82ga
0.18)
99.8(HoEr)
0.2
Except in batching step, the Er taking Ho and 0.1g of Ga, 0.099g of Fe, 7.55g of 27.3g is for subsequent use; Prepare in magnetostriction materials step, adopt Fe
82ga
18graphite heating body as seed crystal, and is heated to 1650 DEG C by single crystal seed, and control temperature gradient is 3 × 10 in addition
5k/m, the speed of growth is outside 4000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.82ga
0.18)
99.8(HoEr)
0.2magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.82ga
0.18)
99.8(HoEr)
0.2magnetostriction materials are the monocrystal material of <100> orientation; In addition, should (Fe
0.82ga
0.18)
99.8(HoEr)
0.2the saturation magnetostriction constant of material is 1120ppm, and saturation magnetic field is about 490Oe, Magnetostriction and comprehensive usability good.
Embodiment 8 prepares (Fe
0.83ga
0.17)
99.84(SmTm)
0.16
Except in batching step, the Tm taking Sm and 0.084g of Ga, 0.075g of Fe, 7.33g of 28.39g is for subsequent use; Prepare in magnetostriction materials step, graphite heating body is heated to 1650 DEG C, and control temperature gradient is 2 × 10
5k/m, the speed of growth is outside 10000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.83ga
0.17)
99.84(SmTm)
0.16magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.83ga
0.17)
99.84(SmTm)
0.16in magnetostriction materials, Sm and Tm element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.83ga
0.17)
99.84(SmTm)
0.16the saturation magnetostriction constant of material is 998ppm, and saturation magnetic field is about 500Oe, Magnetostriction and comprehensive usability good.
Embodiment 9 prepares (Fe
0.82ga
0.18)
99.85(HoErTm)
0.15
Except in batching step, the Tm taking Er and 0.053g of Ho, 0.052g of Ga, 0.052g of Fe, 7.63g of 28.53g is for subsequent use; Prepare in magnetostriction materials step, adopt Fe
82.5ga
17.5graphite heating body as seed crystal, and is heated to 1675 DEG C by single crystal seed, and control temperature gradient is 5 × 10 in addition
5k/m, the speed of growth is outside 3000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.82ga
0.18)
99.85(HoErTm)
0.15magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.82ga
0.18)
99.85(HoErTm)
0.15in magnetostriction materials, Ho, Er and Tm element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.82ga
0.18)
99.85(HoErTm)
0.15the saturation magnetostriction constant of material is 1015ppm, and saturation magnetic field is about 500Oe, Magnetostriction and comprehensive usability good.
Embodiment 10 prepares (Fe
0.81ga
0.19)
99.85(TbDyHo)
0.15
Except in batching step, the Ho taking Dy and 0.051g of Tb, 0.05g of Ga, 0.049g of Fe, 8.26g of 27.92g is for subsequent use; Prepare in magnetostriction materials step, adopt Fe
81ga
19graphite heating body as seed crystal, and is heated to 1650 DEG C by single crystal seed, and control temperature gradient is 1 × 10 in addition
5k/m, the speed of growth is outside 15000mm/h, and other step is identical with embodiment 1, and obtained composition is (Fe
0.81ga
0.19)
99.85(TbDyHo)
0.15magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.81ga
0.19)
99.85(TbDyHo)
0.15in magnetostriction materials, Tb, Dy and Ho element is solidly soluted in FeGa matrix completely, and material is the monocrystal material of <100> orientation; In addition, should (Fe
0.81ga
0.19)
99.85(TbDyHo)
0.15the saturation magnetostriction constant of material is 1300ppm, and saturation magnetic field is about 490Oe, Magnetostriction and comprehensive usability good.
Comparative example 1
The mother alloy rod obtained to embodiment 1 cleans, and obtains washed samples.Washed samples is put into the alumina crucible of directional solidification furnace, 3.0 × 10 are evacuated to directional solidification furnace
-3after Pa, in body of heater, be filled with the high-purity argon gas that purity is more than 99.99%, treat that in stove, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later, repeatedly after this step operation three times, mother alloy rod is heated to molten state at about 1600 DEG C.
Control temperature gradient is 1 × 10
2k/m, the speed of growth is 500mm/h, by the material of melting reposefully pull in GaIn alloy, carry out single crystal growing when directional freeze; After growth terminates, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, obtained composition is (Fe
0.83ga
0.17)
99.95tb
0.05magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe
0.83ga
0.17)
99.95tb
0.05in magnetostriction materials, Tb element is not solidly soluted in FeGa matrix completely, but be pinned at grain boundaries to separate out, and this material is the polycrystalline material of <100> and <110> orientation; In addition, should (Fe
0.83ga
0.17)
99.95tb
0.05the saturation magnetostriction constant of material is about 300ppm, and the performance of material does not significantly improve.
Last it is noted that above each embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to foregoing embodiments to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein some or all of technical characteristic; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (10)
1. magnetostriction materials, is characterized in that, its composition is (Fe
1-xga
x)
100-yrE
y, wherein 0.17≤x≤0.19,0.01≤y≤0.2, RE be selected from Tb, La, Sm, Dy, Lu, Ho, Er and Tm one or more.
2. magnetostriction materials according to claim 1, is characterized in that, its composition is (Fe
0.83ga
0.17)
99.95tb
0.05, (Fe
0.83ga
0.17)
99.95sm
0.05, (Fe
0.83ga
0.17)
99.95dy
0.05, (Fe
0.83ga
0.17)
99.95ho
0.05, (Fe
0.83ga
0.17)
99.95er
0.05, (Fe
0.83ga
0.17)
99.95tm
0.05, (Fe
0.81ga
0.19)
99.95tb
0.05, (Fe
0.81ga
0.19)
99.95sm
0.05, (Fe
0.81ga
0.19)
99.95dy
0.05, (Fe
0.81ga
0.19)
99.95ho
0.05, (Fe
0.81ga
0.19)
99.95er
0.05, (Fe
0.81ga
0.19)
99.95tm
0.05, (Fe
0.83ga
0.17)
99.97lu
0.03, (Fe
0.81ga
0.19)
99.96dy
0.04, (Fe
0.82ga
0.18)
99.98sm
0.02, (Fe
0.81ga
0.19)
99.9tm
0.1, (Fe
0.81ga
0.19)
99.8la
0.2, (Fe
0.82ga
0.18)
99.8(HoEr)
0.2, (Fe
0.83ga
0.17)
99.84(SmTm)
0.16, (Fe
0.82ga
0.18)
99.85(HoErTm)
0.15or (Fe
0.81ga
0.19)
99.85(TbDyHo)
0.15.
3. magnetostriction materials according to claim 1, is characterized in that, it is the monocrystal material of <100> orientation.
4. the preparation method of the arbitrary described magnetostriction materials of claims 1 to 3, is characterized in that, comprise the steps:
1) Fe, Ga and RE raw material is equipped with according to the component requirements of magnetostriction materials;
2) Fe, Ga and RE raw material of outfit is smelted into mother alloy ingot;
3) described mother alloy ingot is melted, and make mother alloy rod by suction pouring;
4) the FeGa single crystal seed of described mother alloy rod and <100> orientation is placed in apparatus for directional solidification; and make FeGa single crystal seed bottom immerse cooling fluid; apparatus for directional solidification to be vacuumized and after being filled with shielding gas; heating makes the complete melting of mother alloy rod and the top melting of FeGa single crystal seed; the material of melting is carried out directional freeze in the pull to cooling fluid of FeGa single crystal seed bottom, and the thermograde controlling described directional freeze is 1 × 10
5~ 9 × 10
5k/m, the speed of growth is 1000 ~ 20000mm/h, obtained described magnetostriction materials.
5. preparation method according to claim 4, is characterized in that, step 4) in, apparatus for directional solidification is vacuumized and is filled with shielding gas and comprise and implement following operation at least one times:
1.0 × 10 are evacuated to apparatus for directional solidification
-3~ 5.0 × 10
-3be filled with shielding gas after Pa, treat that the vacuum tightness in apparatus for directional solidification rises to 1.0 × 10
-1~ 5 × 10
-1inflation is stopped after Pa.
6. the preparation method according to claim 4 or 5, it is characterized in that, step 4) in, described mother alloy rod and FeGa single crystal seed top are placed in the inside of hollow graphite heating member, described graphite heating body is heated, to make the complete melting of mother alloy rod and the top melting of FeGa single crystal seed by ruhmkorff coil.
7. preparation method according to claim 6, is characterized in that, step 4) in, described heating comprises implements following operation at least one times:
With the heat-up rate of 30 ~ 40 DEG C/min, graphite heating body is heated to 1550 ~ 1700 DEG C, insulation 5 ~ 15min after mother alloy rod and the top melting of FeGa single crystal seed, then with the cooling rate of 20 ~ 30 DEG C/min graphite heating body be cooled to 1450 ~ 1550 DEG C and be incubated 3 ~ 8min, then with the heat-up rate of 30 ~ 40 DEG C/min graphite heating body be heated to 1550 ~ 1700 DEG C and be incubated 5 ~ 15min.
8., according to the arbitrary described preparation method of claim 4 to 7, it is characterized in that, step 4) in, make FeGa single crystal seed bottom immerse cooling fluid and lower end in contact water-cooled metal part, described cooling fluid is Ga-In alloy.
9., according to the arbitrary described preparation method of claim 4 to 8, it is characterized in that, step 2) comprising:
Fe, Ga and RE raw material of outfit is placed in melting equipment, 5.0 × 10 are evacuated to melting equipment
-2~ 5.0 × 10
-3be filled with shielding gas after Pa, treat that the vacuum tightness in melting equipment rises to 1.0 × 10
-1~ 5.0 × 10
-1after Pa stop inflation, implement aforesaid operations at least one times after, at melting electric current be under the condition of 100 ~ 150A melting raw material once more than, the time controlling each melting is 3 ~ 5 minutes, makes mother alloy ingot.
10., according to the arbitrary described preparation method of claim 4 to 8, it is characterized in that, step 3) comprising:
Described mother alloy ingot is placed in melting equipment, 1.0 × 10 are evacuated to melting equipment
-3~ 5.0 × 10
-3be filled with shielding gas after Pa, treat that the vacuum tightness in melting equipment rises to 1.0 × 10
-1~ 5.0 × 10
-1stopping inflation after Pa, is, under the condition of 100 ~ 300A, described mother alloy ingot is fused into aluminium alloy at melting electric current, and aluminium alloy suction casting is made mother alloy rod to mould.
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