CN104947194B - A kind of magnetostriction materials and preparation method thereof - Google Patents
A kind of magnetostriction materials and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of magnetostriction materials and preparation method thereof.The magnetostriction materials composition is (Fe1‑xGax)100‑yREy, wherein the one or more of 0.17≤x≤0.19,0.01≤y≤0.2, RE in Tb, La, Sm, Dy, Lu, Ho, Er and Tm.After Fe, Ga and RE for being equipped with according to component requirements are smelted into mother alloy ingot and foundry alloy rod is made, by foundry alloy rod and<100>The FeGa single crystal seeds of orientation are placed in apparatus for directional solidification; after being vacuumized to apparatus for directional solidification and being filled with protective gas; heating makes the melting completely of foundry alloy rod and FeGa single crystal seeds top melts; the material of melting is oriented solidification into coolant along FeGa single crystal seeds bottom pull, and it is 1 × 10 to control thermograde5~9 × 105K/m, the speed of growth are 1000~20000mm/h.This method prepare magnetostriction materials be<100>The monocrystal material of orientation, rare earth element are dissolved into FeGa matrixes completely, and its saturation magnetic field is only 100~500Oe, and magnetostriction coefficient is up to 300~1500ppm, and comprehensive usability is good, has a extensive future.
Description
Technical field
The present invention relates to a kind of magnetic material, more particularly to a kind of magnetostriction materials and preparation method thereof.
Background technology
Magnetostriction materials can exist as a kind of important ferromagnetic functional material, its physical dimension with the change of magnetized state
Reversible change occurs for all directions, and the reversible deformation of this Magnetic Field-Induced is referred to as magnetostriction.Magnetic is proposed from joule in 1842
Since causing flex effect, it is all that magnetostriction materials are just widely applied to aviation, navigation, robot, new energy, biomedicine etc.
It is multi-field, played an important role in national economy and industrial production.Magnetostriction material of the FeGa alloys as latest generation
Material, the good synthesis performance so that saturation magnetic field is low, mechanical property is good, magnetostriction is big etc. and by extensive concern, turn into two
The strategic new material of eleventh century.
Although the synthesis performance of FeGa alloys is good, but traditional FeGa bianry alloy saturation magnetostriction constants
Only the 1/5 of Terfenol-D alloys, therefore it is prepared by optimize technique<100>The monocrystal material and design alloying component of orientation make
FeGa matrixes have bigger magnetostriction coefficient, turn into the inevitable choice for further improving FeGa matrix Magnetostrictions.
At present, the research both at home and abroad for FeGa alloys is also concentrated mainly on raising Magnetostriction and optimization material preparation process
On.
Publication No. CN101086912A Chinese patent discloses a kind of FeGa-RE series magnetostriction materials and its manufacture
Technique, the magnetostriction materials are polycrystal.Its main component is Fe, Ga and RE, wherein adding La, Ce, Pr, Nd, Tb, Dy
In one or more, content 0.01-20at%.The manufacturing process of the magnetostriction materials is included after raw material is refined
Alloy pour into required for pole, to alloy bar high-temperature gradient rapid solidification method or czochralski method or Bridgman methods,
Epitaxis is carried out, is finally given<100>With<110>The magnetostriction materials of orientation.However, the magnetostriction of the material
Coefficient is only 300ppm or so, and the material Magnetostriction prepared using the method is not obviously improved, and its reason may
It is being that precipitation is pinned at grain boundaries and is not dissolved into FeGa matrixes in the form of the second phase in rare earth atom.
Publication No. CN103556045A Chinese patent discloses one kind and is based on FeGa-RFe2Magnetocrystalline anisotropy compensates
New Magnetostrictive Material of principle design and preparation method thereof, the composition of the magnetostriction polycrystalline material is (Fe100-XGaX)Y
(RFe2)Z, wherein compensating the ratio Y of composition in 10≤X≤40, Y and Z regulation pseudo-binary system:Z=1~20, RFe2For TbFe2、
SmFe2、DyFe2、HoFe2、ErFe2、TmFe2In one or several kinds.The patent in FeGa alloys by adding Tb, Sm etc.
Rare earth element, and prepared using vacuum belt-rejecting technology<100>The single phase homogeneous polycrystalline band of orientation.However, vacuum gets rid of band work
Polycrystalline beam thickness prepared by skill is only tens microns, and Tape samples cause low field due to special shape anisotropy
(＜ 500Oe) Magnetostriction extreme difference (＜ 50ppm), it is impossible to meet the magnetostrictive devices such as high-power transducer for low field
The use demand of high performance three-dimensional crystalline material.
The content of the invention
The present invention provides a kind of magnetostriction materials, and it is<100>The monocrystal material of orientation, and material rare earth elements
It is dissolved into completely in FeGa matrixes, not only magnetostriction coefficient significantly improves, and saturation magnetic field is relatively low in addition, comprehensive usability
It is good.
The present invention also provides a kind of preparation method of magnetostriction materials, and its is simple to operate, technique is easily controllable, and energy
The Magnetostriction magnetostriction materials good with comprehensive usability are enough made.
The present invention provides a kind of magnetostriction materials, and its composition is (Fe1-xGax)100-yREy, wherein 0.17≤x≤0.19,
The one or more of 0.01≤y≤0.2, RE in Tb, La, Sm, Dy, Lu, Ho, Er and Tm.
Further, the composition of the magnetostriction materials is (Fe0.83Ga0.17)99.95Tb0.05、(Fe0.83Ga0.17)99.95Sm0.05、(Fe0.83Ga0.17)99.95Dy0.05、(Fe0.83Ga0.17)99.95Ho0.05、(Fe0.83Ga0.17)99.95Er0.05、
(Fe0.83Ga0.17)99.95Tm0.05、(Fe0.81Ga0.19)99.95Tb0.05、(Fe0.81Ga0.19)99.95Sm0.05、(Fe0.81Ga0.19)99.95Dy0.05、(Fe0.81Ga0.19)99.95Ho0.05、(Fe0.81Ga0.19)99.95Er0.05、(Fe0.81Ga0.19)99.95Tm0.05、
(Fe0.83Ga0.17)99.97Lu0.03、(Fe0.81Ga0.19)99.96Dy0.04、(Fe0.82Ga0.18)99.98Sm0.02、(Fe0.81Ga0.19)99.9Tm0.1、(Fe0.81Ga0.19)99.8La0.2、(Fe0.82Ga0.18)99.8(HoEr)0.2、(Fe0.83Ga0.17)99.84(SmTm)0.16、
(Fe0.82Ga0.18)99.85(HoErTm)0.15Or (Fe0.81Ga0.19)99.85(TbDyHo)0.15。
Further, the magnetostriction materials are<100>The monocrystal material of orientation.Particularly, the magnetostriction material
Material has (200) diffraction maximum between being 27 °~28 ° in 2 θ, and has (400) diffraction maximum between being 56 °~57 ° in 2 θ；This
Outside, the weight symmetry of magnetostriction materials difference family of crystal planes diffraction spot four.
Further, in the magnetostriction materials, RE is dissolved completely in FeGa matrixes.The present invention is to described completely solid
Molten not strict limitation, wherein the situation being substantially completely dissolved can also be included.Specifically, can be by not having on BSE images
Or the pattern for not having RE element precipitated phases substantially proves that RE is dissolved completely in FeGa matrixes.
Further, there is a plurality of dislocation line in the magnetostriction materials.Particularly, at least two in a plurality of dislocation line
Dislocation line, which is formed, to intersect；Especially, a plurality of dislocation line intersects at one and forms the radioactive ray radiated at this to surrounding
Shape.The length of the dislocation line can be 30~150nm.
Further, the saturation magnetic field of the magnetostriction materials is 100~500Oe, for example, 300~500Oe, preferably
For 300~400Oe, more preferably 300~350Oe.
Further, the saturation magnetostriction constant of the magnetostriction materials is 300~1500ppm, preferably 450~
1500ppm, more preferably 650~1500ppm, it is still more preferably 1000~1500ppm.
Further, the magnetostriction materials are club-shaped material, and its a diameter of 1~10mm, length is 1~20mm, excellent
Elect 5~10mm of diameter, 10~20mm of length as.
The present invention also provides a kind of preparation method of any of the above-described described magnetostriction materials, comprises the following steps：
1) Fe, Ga and RE raw material are equipped with according to the component requirements of magnetostriction materials；
2) Fe, Ga and RE raw material of outfit are smelted into mother alloy ingot；
3) mother alloy ingot is melted, and foundry alloy rod is made by suction pouring；
4) by the foundry alloy rod and<100>The FeGa single crystal seeds of orientation are placed in apparatus for directional solidification, and make FeGa
Coolant is immersed in single crystal seed bottom, and after being vacuumized to apparatus for directional solidification and being filled with protective gas, heating makes foundry alloy rod complete
Full-fusing and FeGa single crystal seeds top melt, by the material of melting along FeGa single crystal seeds bottom pull into coolant
Be oriented solidification, and control the directional solidification thermograde be 1 × 105~9 × 105K/m, the speed of growth 1000
~20000mm/h, the magnetostriction materials are made.
In the present invention, directional solidification is referred in frozen metal (i.e. non-molten metal) and non-frozen metal molten mass
The thermograde (G) of specific direction is established, a kind of casting technique for making molten mass be solidified along the direction opposite with hot-fluid；Growth
Speed is referred to the speed of molten mass pull into coolant.Special rare earth elements selected by the present invention have large scale and
Big magnetocrystalline anisotropy, while be oriented solidification under above-mentioned specific thermograde and the speed of growth and be advantageously implemented rare earth
The single-crystal orientation of complete solid solution and magnetostriction materials of the element in FeGa matrixes.Further, thermograde is preferably 1
×105~5 × 105K/m；The speed of growth (V) is preferably 1000~10000mm/h, more preferably 2000~8000mm/h.
The present invention uses in directional solidification<100>FeGa single crystal seeds are orientated as seed crystal, and are using the seed crystal
When become partially molten state；Specifically, coagulate by way of controlling heating and cooling the melting of seed crystal top, bottom
Gu so as to make solid liquid interface in solid-liquid phase-change process be promoted along seed crystal bottom in directional solidification, it is orientated the advantage of seed crystal
It is retained, so that lattice stacking of the crystal newly formed along seed crystal, it is easier to crystal growth；In addition, by growing faster
Speed (more than 1000mm/h) makes solid liquid interface be put down by concave change, while higher thermograde (1 × 105More than K/m) suppress shape
Core, ultimately result in monocrystalline and grow up, so as to realize complete solid solution and magnetostriction materials of the rare earth element in FeGa matrixes<
100>Single-crystal orientation.
Raw material Fe, Ga and RE that the present invention selects purity are all higher than 99.99wt%.
In the step 4) of the present invention, apparatus for directional solidification, which is vacuumized, and is filled with protective gas includes implementing following operate
At least once：
1.0 × 10 are evacuated to apparatus for directional solidification-3~5.0 × 10-3Protective gas is filled with after Pa, treats directional solidification
Vacuum in equipment rises to 1.0 × 10-1~5 × 10-1Stop inflation after Pa.
Preferably, aforesaid operations are implemented three to four times.
Further, in step 4) of the present invention, the foundry alloy rod and FeGa single crystal seeds top are placed in hollow graphite
The inside of calandria, the graphite heating body is heated by induction coil, so that foundry alloy rod melting and FeGa monocrystalline completely
Seed crystal top melts.
Graphite heating body is heated to specify by above-mentioned mode of heating by being arranged on the induction coil on the outside of graphite heating body
After temperature, heat release is carried out to the material being provided at its inner portion by the heat radiation of graphite heating body, so as to realize to material
Heating.The mode of heating is easy to be heated evenly material, and can realize larger temperature, less radial symmetry gradient etc.,
Be advantageous to the single-crystal orientation of material.
Further, in step 4) of the present invention, the heating includes implementing following operation at least once：
Graphite heating body is heated to 1550~1700 DEG C with 30~40 DEG C/min programming rate, treat foundry alloy rod and
5~15min is incubated after the melting of FeGa single crystal seeds top, is then dropped graphite heating body with 20~30 DEG C/min cooling rate
Temperature is to 1450~1550 DEG C and is incubated 3~8min, then is heated to graphite heating body with 30~40 DEG C/min programming rate
1550~1700 DEG C and 5~15min of insulation.
In the present invention, the temperature of material is made to exceed more than 50~200 DEG C of its melting temperature by heating, and using upper
State ad hoc fashion to carry out heating and not only contribute to material fully melting, also help the passivation and mistake of heterogeneous forming core in molten mass
Effect, so as to reduce the heterogeneous forming core in molten mass, and is advantageous to the single-crystal orientation of material.Preferably, implement aforesaid operations three to
Four times.
In addition, in step 4), FeGa single crystal seeds bottom is set to immerse coolant and lower end in contact water-cooled metal part, it is described
Coolant is Ga-In alloys.
That is, the present invention can be by heating, while to FeGa single crystal seeds to FeGa single crystal seeds top
The mode that bottom is cooled down realizes the partially molten state of seed crystal.Particularly, in directional solidification, using Ga-In alloy (liquid
State metal coolant) and the mode that is combined of water-cooled metal part cooled down, wherein being entered using Ga-In alloys to the side of material
Row cooling, while the lower end of material is cooled down using water-cooled metal part, which is easily achieved larger thermograde, together
The more preferable axial cooling effects of Shi Shixian.Water-cooled metal part refers to the metal portion cooled down using water as cooling medium
Part, structure and material to metal parts do not limit strictly, such as can be water-cooled copper fixture.
Further, step 2) includes：
Fe, Ga and RE raw material of outfit are placed in smelting equipment, 5.0 × 10 are evacuated to smelting equipment-2~5.0 ×
10-3Protective gas is filled with after Pa, treats that the vacuum in smelting equipment rises to 1.0 × 10-1~5.0 × 10-1Stop filling after Pa
Gas, implement aforesaid operations at least once after, melting electric current be 100~150A under conditions of melting raw material once more than, control
The time of each melting is 3~5 minutes, and mother alloy ingot is made.
Preferably, melting raw material three to five times under these conditions.
Further, step 3) includes：
The mother alloy ingot is placed in smelting equipment, 1.0 × 10 are evacuated to smelting equipment-3~5.0 × 10- 3Protective gas is filled with after Pa, treats that the vacuum in smelting equipment rises to 1.0 × 10-1~5.0 × 10-1Stop inflation after Pa,
Aluminium alloy is inhaled casting to mould by melting electric current for the mother alloy ingot is fused into aluminium alloy under conditions of 100~300A
In foundry alloy rod is made.
In concrete scheme of the present invention, the smelting equipment can be the conventional equipment of this area, such as vacuum non-consumable
Arc-melting furnace；The protective gas can be argon gas of purity more than 99.99% etc..
The implementation of the present invention, at least has the advantage that：
1st, the present invention in FeGa matrixes by adding the micro member of the rare earth with large scale and big magnetocrystalline anisotropy
Element, in combination with the directional solidification processes with higher thermograde and the faster speed of growth, it is achieved thereby that rare earth is first
Complete solid solution and magnetostriction materials of the element in FeGa matrixes<100>Single-crystal orientation.
2nd, preparation method of the invention is simple to operate, technique is easily controllable, rare earth element addition is few, short preparation period,
Particularly specific mode of heating be advantageous to material fully melt and molten mass in heterogeneous forming core passivation and failure, specifically
The type of cooling is easily obtained larger thermograde, good cooling results, the Magnetostriction of obtained magnetostriction materials and
Comprehensive usability is good, applied widely.
3rd, the magnetostriction materials prepared by preparation method of the present invention are<100>The monocrystal material of orientation, in the material
Rare earth element is dissolved into FeGa matrixes completely, and saturation magnetic field is only 100~500Oe, and magnetostriction coefficient is up to 300~
1500ppm, comprehensive usability is good, has a extensive future.
Brief description of the drawings
Fig. 1 is the BSE images of mother alloy ingot prepared by the embodiment of the present invention 1；
Fig. 2 is the XRD spectrum of foundry alloy rod prepared by the embodiment of the present invention 1；
Fig. 3 is the BSE images of magnetostriction materials prepared by the embodiment of the present invention 1；
Fig. 4 is the synchrotron radiation X RD collection of illustrative plates and Laue diffracting spectrums 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 uses83Ga17The 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 uses83Ga17The magnetostriction of single crystal seed and the magnetostriction materials of preparation
Curve.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, accompanying drawing and implementation below in conjunction with the present invention
Example, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention
Part of the embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
The every other embodiment obtained under the premise of creative work is made, belongs to the scope of protection of the invention.
Embodiment 1 prepares (Fe0.83Ga0.17)99.95Tb0.05
Prepared composition is (Fe0.83Ga0.17)99.95Tb0.05Magnetostriction materials method, comprise the following steps：
1st, dispensing
Raw material Fe, Ga and Tb (RE raw materials) of selection purity are all higher than 99.99wt%, and in order to prevent fusion process
Middle melting loss of elements, according to mentioned component be equipped with Fe, Ga and Tb raw material when, according to about 1wt% scaling loss amount add respectively Ga and
Tb.Specifically, 27.72g Fe, 7.158g Ga and 0.048g Tb are weighed, it is standby.
2nd, 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, will when placing
The metallic element of easy scaling loss is placed in crucible bottom, and the metallic element being unlikely to be burnt is placed in above crucible.
Vacuum non-consumable arc-melting furnace is carried out being evacuated to 4.0 × 10-3After Pa, high-purity argon gas is filled with into body of heater,
The volumn concentration (purity) of argon gas is more than 99.99%, treats that the vacuum in stove rises to 1.0 × 10-1Stop after Pa
Inflation, repeatedly this step operation three times after, melting electric current is arranged to 150A, to raw material carry out melting, control each melting when
Between be 4 minutes or so, melt back four times, be made mother alloy ingot, to the mother alloy ingot carry out electron probe test, its carry on the back
Scattered electron (BSE) image is as shown in Figure 1；From fig. 1, it can be seen that Tb elements are with the second phase in mother alloy ingot material under as cast condition
Form is distributed widely in FeGa matrix grain boundaries.
3rd, foundry alloy rod is prepared
Master alloy ingot obtained above is placed in vacuum non-consumable arc-melting furnace, to vacuum non-consumable arc-melting furnace
It is evacuated to 3.0 × 10-3After Pa, the high-purity argon gas that volumn concentration is more than 99.99% is filled with into body of heater, is treated true in stove
Reciprocal of duty cycle rises to 1.0 × 10-1Pa stops inflating later.
Melting electric current is arranged to 150A, master alloy melting ingot, rapidly by melting electric current when master alloy ingot soon melts
Regulation is to 300A, arc blow-out at alignment master alloy ingot center, mould hole, while opens suction pouring valve, using negative pressure by wink
Between the foundry alloy liquid that melts inhale to cast onto foundry alloy rod be made in mould, its XRD spectrum is as shown in Figure 2；As a result show：The foundry alloy
Rod is polycrystalline tissue, polycrystalline orientation with<110>、<100>Based on.
4th, magnetostriction materials are prepared
By foundry alloy rod outer surface grinding homogeneity obtained above, with<100>The Fe of orientation83Ga17Single crystal seed is together soaked
Steep in acetone, 10min is cleaned by ultrasonic under 50KHz frequency, is put in after cleaning in baking oven, dry 20min in 120 DEG C, obtain
Obtain washed samples.
Solidification is oriented to material using directional solidification furnace, graphite heating body is placed on insulation ring first, and will
Insulation ring is placed on GaIn alloy tanks；Secondly washed samples are put into alumina crucible, when placing, foundry alloy rod put
Put in Fe83Ga17The top of single crystal seed, and by crucible be positioned over inside cylindrical hollow graphite heating body center and
The top of GaIn alloy tanks；Crucible is fallen into GaIn alloy tanks again, makes the Fe in crucible83Ga17The bottom of single crystal seed is immersed
GaIn alloys in GaIn alloy tanks simultaneously make Fe83Ga17The contact surface of single crystal seed and foundry alloy rod is located at the liquid level of GaIn alloys
Top；Meanwhile water-cooled copper fixture is set below seed crystal, and the lower end of seed crystal is formed with water-cooled copper fixture and contact, water-cooled copper
Fixture carries out circulating cooling using 5 DEG C or so of cold water.
Then, 3.0 × 10 are evacuated to directional solidification furnace-3After Pa, into body of heater being filled with volumn concentration is
More than 99.99% high-purity argon gas, treat that vacuum rises to 1.0 × 10 in stove-1Pa stops inflating later, repeatedly this step operation three
After secondary, graphite heating body is heated to 1600 DEG C with 35 DEG C/min programming rate, treat foundry alloy rod completely melting and
Fe83Ga1710min is incubated after the melting of single crystal seed top, then with 25 DEG C/min cooling rate by the temperature of graphite heating body
1500 DEG C are down to, is incubated 5min at such a temperature, then graphite heating body is heated to 1600 DEG C with identical programming rate and protected
Warm 10min, operation is incubated 30min, foundry alloy rod melting and Fe completely afterwards three times above for circulation83Ga17Single crystal seed turns into upper
Portion's melting, the partially molten state of bottom solidification.
It is 1 × 10 to control thermograde5K/m, speed of growth 20000mm/h, by the material of melting along FeGa monocrystalline
Smoothly downward pull is oriented solidification into GaIn alloys for seed crystal bottom, during directional solidification, passes through GaIn alloy coolants
Material side is cooled down, while material lower end cooled down by water-cooled copper fixture, makes crystal growth；End to be grown
Afterwards, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, it is (Fe that composition, which is made,0.83Ga0.17)99.95Tb0.05Bar-shaped magnetic
Cause telescopic material (size Φ 7mm × 20mm), its BSE image and synchrotron radiation X RD collection of illustrative plates with Laue diffracting spectrums respectively such as Fig. 3
Shown in Fig. 4, Fig. 3 shows do not have RE element precipitated phases in the magnetostriction materials, and Fig. 4 shows that the magnetostriction materials are in 2 θ
There is (200) diffraction maximum between 27 °~28 °, and there is (400) diffraction maximum between being 56 °~57 ° in 2 θ, in addition, the mangneto
The weight symmetry of telescopic material difference family of crystal planes diffraction spot four.Thus illustrate：Should (Fe0.83Ga0.17)99.95Tb0.05Magnetostriction materials
Middle Tb elements are dissolved into FeGa matrixes completely, and material is<100>The monocrystal material of orientation.
Respectively to Fe83Ga17Single crystal seed and the (Fe prepared0.83Ga0.17)99.95Tb0.05Magnetostriction materials are transmitted
Electronic Speculum is tested, edge<100>Dark field image under crystal zone axis observation material STEM patterns, as a result as shown in Figure 5 and Figure 6.As a result show：
Common Fe83Ga17Monocrystalline interior microscopic even tissue is consistent (Fig. 5), and (the Fe prepared0.83Ga0.17)99.95Tb0.05In material
Substantially it is observed that substantial amounts of dislocation line, a plurality of dislocation line intersect at one and formed and put at this to what surrounding radiated
Aplysia punctata, and the length of dislocation line is 30~150nm, and reason may is that the solid solution of Tb elements causes FeGa matrixes to produce four
Side's distortion, distortion cause to generate internal stress in matrix material, and internal stress is showed by the form of dislocation line.
In addition, measured using magnetostriction measurement system (Beijing WuKe opto-electrical Technology Co., Ltd's production)
(Fe0.83Ga0.17)99.95Tb0.05Material and Fe83Ga17The magnetostrictive strain value of monocrystalline, wherein foil gauge use Japanese republicanism
KFG-1-120-C1-11L3M2R type resistance strain gages, as a result as shown in Figure 7.As a result show：(Fe0.83Ga0.17)99.95Tb0.05Material
The saturation magnetostriction constant of material is 463ppm, and it compares Fe83Ga17The magnetostriction coefficient of monocrystalline improves 50% or so；This
Outside, (Fe0.83Ga0.17)99.95Tb0.05The saturation magnetic field of material is only 300Oe or so, and Magnetostriction and comprehensive usability are good
It is good.
Embodiment 2 prepares (Fe0.83Ga0.17)99.97Lu0.03
Except Fe, the 7.242g in batching step, weighing 28.05g Ga and 0.031g Lu are standby；Prepare magnetostriction material
Expect in step, graphite heating body is heated to 1575 DEG C, and it is 5 × 10 to control thermograde5K/m, speed of growth 8000mm/
Outside h, other steps are same as Example 1, and it is (Fe that composition, which is made,0.83Ga0.17)99.97Lu0.03Magnetostriction materials (size
Φ7mm×20mm)。
After testing, should (Fe0.83Ga0.17)99.97Lu 0.03Lu elements are dissolved into FeGa matrixes completely in magnetostriction materials
In, and material is<100>The monocrystal material of orientation；In addition, should (Fe0.83Ga0.17)99.97Lu0.03The saturation magnetostriction of material
Coefficient is 330ppm, and saturation magnetic field is 350Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 3 prepares (Fe0.81Ga0.19)99.96Dy0.04
Prepared composition is (Fe0.81Ga0.19)99.96Dy0.04Magnetostriction materials method, comprise the following steps：
1st, dispensing
27.88g Fe, 8.25g Ga and 0.04g Dy are weighed, it is standby.
2nd, 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, it is non-to vacuum from
Consumption arc-melting furnace carries out being evacuated to 1.0 × 10-3After Pa, the high-purity argon gas that purity is more than 99.99% is filled with into body of heater,
Treat that the vacuum in stove rises to 5.0 × 10-1Pa stops inflating later, and repeatedly after this step operation three times, melting electric current is set
For 120A, melting is carried out to raw material, the time for controlling each melting is 5 minutes or so, melt back four times, and foundry alloy casting is made
Ingot.
3rd, foundry alloy rod is prepared
Master alloy ingot obtained above is placed in vacuum non-consumable arc-melting furnace, to vacuum non-consumable arc-melting furnace
It is evacuated to 1.0 × 10-3After Pa, the high-purity argon gas that purity is more than 99.99% is filled with into body of heater, treats that vacuum rises in stove
To 5.0 × 10-1Pa stops inflating later.
Melting electric current is arranged to 120A, master alloy melting ingot, rapidly by melting electric current when master alloy ingot soon melts
Regulation is to 300A, arc blow-out at alignment master alloy ingot center, mould hole, while opens suction pouring valve, using negative pressure by wink
Between the foundry alloy liquid that melts inhale to cast onto foundry alloy rod be made in mould, the foundry alloy rod be polycrystalline tissue, polycrystalline be orientated with<110
>、<100>Based on.
4th, magnetostriction materials are prepared
To foundry alloy rod obtained above and<100>The Fe of orientation81Ga19Single crystal seed is cleaned, and obtains cleaning examination
Sample.
Solidification is oriented to material using directional solidification furnace, it is solidifying to orienting after placing good material according to the method for embodiment 1
Gu stove evacuation is to 1.0 × 10-3Pa, the high-purity argon gas that purity is more than 99.99% is filled with into body of heater, is treated in stove in vacuum
Rise to 5.0 × 10-1Stop inflating after Pa, repeatedly after this step operation three times, with 40 DEG C/min programming rate by graphite heating
Body is heated to 1575 DEG C, treats foundry alloy rod melting and Fe completely81Ga19Single crystal seed top melting after be incubated 5min, then with
The temperature of graphite heating body is down to 1500 DEG C by 30 DEG C/min cooling rate, is incubated 3min at such a temperature, then with identical
Graphite heating body is heated to 1575 DEG C and is incubated 5min by programming rate, and more than circulation operation is incubated 30min, foundry alloy afterwards three times
Rod melting and Fe completely81Ga19Single crystal seed turns into top melting, the partially molten state of bottom solidification.
It is 4 × 10 to control thermograde5K/m, speed of growth 5000mm/h, by the material of melting along FeGa monocrystalline seeds
Smoothly downward pull is oriented solidification into GaIn alloys for brilliant bottom, during directional solidification, passes through GaIn alloy coolants pair
Material side is cooled down, while material lower end is cooled down by water-cooled copper fixture, makes crystal growth；End to be grown
Afterwards, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, it is (Fe that composition, which is made,0.81Ga0.19)99.96Dy0.04Mangneto stretch
Compression material (size Φ 7mm × 20mm).
After testing, should (Fe0.81Ga0.19)99.96Dy0.04Dy elements are dissolved into FeGa matrixes completely in magnetostriction materials,
And material is<100>The monocrystal material of orientation；In addition, should (Fe0.81Ga0.19)99.96Dy0.04The saturation magnetostriction system of material
Number is 454ppm, and saturation magnetic field is 300Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 4 prepares (Fe0.82Ga0.18)99.98Sm0.02
Except Fe, the 7.79g in batching step, weighing 28.12g Ga and 0.019g Sm are standby；Prepare magnetostriction material
Expect in step, using Fe82Ga18Single crystal seed is as seed crystal, and it is 10 × 10 to control thermograde5K/m, the speed of growth are
Outside 1000mm/h, other steps are same as Example 1, and it is (Fe that composition, which is made,0.82Ga0.18)99.98Sm0.02Magnetostriction material
Expect (size Φ 7mm × 20mm).
After testing, should (Fe0.82Ga0.18)99.98Sm0.02Sm elements are dissolved into FeGa matrixes completely in magnetostriction materials,
And material is<100>The monocrystal material of orientation；In addition, should (Fe0.82Ga0.18)99.98Sm0.02The saturation magnetostriction system of material
Number is 315ppm, and saturation magnetic field is 400Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 5 prepares (Fe0.81Ga0.19)99.9Tm0.1
Prepared composition is (Fe0.81Ga0.19)99.9Tm0.1Magnetostriction materials method, comprise the following steps：
1st, dispensing
27.76g Fe, 8.21g Ga and 0.105g Tm are weighed, it is standby.
2nd, 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, it is non-to vacuum from
Consumption arc-melting furnace carries out being evacuated to 5.0 × 10-2After Pa, the high-purity argon gas that purity is more than 99.99% is filled with into body of heater,
Treat that the vacuum in stove rises to 1.0 × 10-1Pa stops inflating later, and repeatedly after this step operation three times, melting electric current is set
For 100A, melting is carried out to raw material, the time for controlling each melting is 5 minutes or so, melt back four times, and foundry alloy casting is made
Ingot.
3rd, foundry alloy rod is prepared
Master alloy ingot obtained above is placed in vacuum non-consumable arc-melting furnace, to vacuum non-consumable arc-melting furnace
It is evacuated to 5.0 × 10-2After Pa, the high-purity argon gas that purity is more than 99.99% is filled with into body of heater, treats that vacuum rises in stove
To 1.0 × 10-1Pa stops inflating later.
Melting electric current is arranged to 100A, master alloy melting ingot, rapidly by melting electric current when master alloy ingot soon melts
Regulation is to 300A, arc blow-out at alignment master alloy ingot center, mould hole, while opens suction pouring valve, using negative pressure by wink
Between the foundry alloy liquid that melts inhale to cast onto foundry alloy rod be made in mould, the foundry alloy rod be polycrystalline tissue, polycrystalline be orientated with<110
>、<100>Based on.
4th, magnetostriction materials are prepared
To foundry alloy rod obtained above and<100>The Fe of orientation81Ga19Single crystal seed is cleaned, and obtains cleaning examination
Sample.
Solidification is oriented to material using directional solidification furnace, it is solidifying to orienting after placing good material according to the method for embodiment 1
Gu stove evacuation is to 5.0 × 10-2Pa, the high-purity argon gas that purity is more than 99.99% is filled with into body of heater, is treated in stove in vacuum
Rise to 1.0 × 10-1Stop inflating after Pa, repeatedly after this step operation three times, with 30 DEG C/min programming rate by graphite heating
Body is heated to 1650 DEG C, treats foundry alloy rod melting and Fe completely81Ga1915min is incubated after the melting of single crystal seed top, then
The temperature of graphite heating body is down to 1500 DEG C with 20 DEG C/min cooling rate, is incubated 8min at such a temperature, then with identical
Programming rate graphite heating body is heated to 1650 DEG C and is incubated 15min, more than circulation operation is incubated 35min afterwards three times, female
Alloy bar melting and Fe completely81Ga19Single crystal seed turns into top melting, the partially molten state of bottom solidification.
It is 5 × 10 to control thermograde5K/m, speed of growth 6000mm/h, by the material of melting along FeGa monocrystalline seeds
Smoothly downward pull is oriented solidification into GaIn alloys for brilliant bottom, during directional solidification, passes through GaIn alloy coolants pair
Material side is cooled down, while material lower end is cooled down by water-cooled copper fixture, makes crystal growth；End to be grown
Afterwards, in-furnace temperature is down to room temperature, takes out the monocrystalline after growth, it is (Fe that composition, which is made,0.81Ga0.19)99.9Tm0.1Magnetostriction
Material (size Φ 7mm × 20mm).
After testing, should (Fe0.81Ga0.19)99.9Tm0.1Tm elements are dissolved into FeGa matrixes completely in magnetostriction materials,
And material is<100>The monocrystal material of orientation；In addition, should (Fe0.81Ga0.19)99.9Tm0.1The saturation magnetostriction constant of material
For 667ppm, saturation magnetic field is 370Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 6 prepares (Fe0.81Ga0.19)99.8La0.2
Except Fe, 8.15g in batching step, weighing 27.55g Ga, 0.086g La are standby；Prepare magnetostriction materials
In step, using Fe81Ga19Single crystal seed is heated to 1650 DEG C as seed crystal, and by graphite heating body, this outer control temperature ladder
Spend for 8 × 105K/m, the speed of growth are that other steps are same as Example 1, and obtained composition is outside 7000mm/h
(Fe0.81Ga0.19)99.8La0.2Magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe0.81Ga0.19)99.8La0.2La elements are dissolved into FeGa matrixes completely in magnetostriction materials,
And material is<100>The monocrystal material of orientation；In addition, should (Fe0.81Ga0.19)99.8La0.2The saturation magnetostriction constant of material
For 1316ppm, saturation magnetic field is 500Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 7 prepares (Fe0.82Ga0.18)99.8(HoEr)0.2
Except Fe, the 7.55g in batching step, weighing 27.3g Ga, 0.099g Ho and 0.1g Er are standby；Prepare magnetic
Cause in telescopic material step, using Fe82Ga18Single crystal seed is heated to 1650 DEG C as seed crystal, and by graphite heating body, in addition
It is 3 × 10 to control thermograde5K/m, the speed of growth are that other steps are same as Example 1 outside 4000mm/h, and composition is made
For (Fe0.82Ga0.18)99.8(HoEr)0.2Magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe0.82Ga0.18)99.8(HoEr)0.2Magnetostriction materials are<100>The monocrystal material of orientation；This
Outside, should (Fe0.82Ga0.18)99.8(HoEr)0.2The saturation magnetostriction constant of material is 1120ppm, and saturation magnetic field is 490Oe left
The right side, Magnetostriction and comprehensive usability are good.
Embodiment 8 prepares (Fe0.83Ga0.17)99.84(SmTm)0.16
Except Fe, the 7.33g in batching step, weighing 28.39g Ga, 0.075g Sm and 0.084g Tm are standby；Prepare
In magnetostriction materials step, graphite heating body is heated to 1650 DEG C, and it is 2 × 10 to control thermograde5K/m, growth speed
Spend for outside 10000mm/h, other steps are same as Example 1, it is (Fe that composition, which is made,0.83Ga0.17)99.84(SmTm)0.16Magnetic
Cause telescopic material (size Φ 7mm × 20mm).
After testing, should (Fe0.83Ga0.17)99.84(SmTm)0.16Sm and Tm elements are dissolved into completely in magnetostriction materials
In FeGa matrixes, and material is<100>The monocrystal material of orientation；In addition, should (Fe0.83Ga0.17)99.84(SmTm)0.16Material
Saturation magnetostriction constant is 998ppm, and saturation magnetic field is 500Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 9 prepares (Fe0.82Ga0.18)99.85(HoErTm)0.15
Except Fe, the 7.63g in batching step, weighing 28.53g Ga, 0.052g Ho, 0.052g Er and 0.053g
Tm is standby；Prepare in magnetostriction materials step, using Fe82.5Ga17.5Single crystal seed adds as seed crystal, and by graphite heating body
For heat to 1675 DEG C, this outer control thermograde is 5 × 105K/m, the speed of growth are outside 3000mm/h, and other steps are with implementing
Example 1 is identical, and it is (Fe that composition, which is made,0.82Ga0.18)99.85(HoErTm)0.15Magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe0.82Ga0.18)99.85(HoErTm)0.15Ho, Er and Tm element are dissolved completely in magnetostriction materials
Into FeGa matrixes, and material is<100>The monocrystal material of orientation；In addition, should (Fe0.82Ga0.18)99.85(HoErTm)0.15Material
The saturation magnetostriction constant of material is 1015ppm, and saturation magnetic field is 500Oe or so, and Magnetostriction and comprehensive usability are good
It is good.
Embodiment 10 prepares (Fe0.81Ga0.19)99.85(TbDyHo)0.15
Except Fe, the 8.26g in batching step, weighing 27.92g Ga, 0.049g Tb, 0.05g Dy and 0.051g
Ho is standby；Prepare in magnetostriction materials step, using Fe81Ga19Single crystal seed heats as seed crystal, and by graphite heating body
To 1650 DEG C, this outer control thermograde is 1 × 105K/m, the speed of growth are other steps and embodiment outside 15000mm/h
1 is identical, and it is (Fe that composition, which is made,0.81Ga0.19)99.85(TbDyHo)0.15Magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe0.81Ga0.19)99.85(TbDyHo)0.15Tb, Dy and Ho element are dissolved completely in magnetostriction materials
Into FeGa matrixes, and material is<100>The monocrystal material of orientation；In addition, should (Fe0.81Ga0.19)99.85(TbDyHo)0.15Material
The saturation magnetostriction constant of material is 1300ppm, and saturation magnetic field is 490Oe or so, and Magnetostriction and comprehensive usability are good
It is good.
Comparative example 1
Foundry alloy rod made from embodiment 1 is cleaned, obtains washed samples.Washed samples are put into directional solidification furnace
Alumina crucible in, 3.0 × 10 are evacuated to directional solidification furnace-3After Pa, be filled with into body of heater purity for 99.99% with
On high-purity argon gas, treat that vacuum rises to 1.0 × 10 in stove-1Pa stops inflating later, repeatedly after this step operation three times, by mother
Alloy bar is heated to molten condition at 1600 DEG C or so.
It is 1 × 10 to control thermograde2K/m, speed of growth 500mm/h, by the material of melting, smoothly pull arrives
In GaIn alloys, crystal growth is carried out in directional solidification；After end to be grown, in-furnace temperature is down to room temperature, takes out growth
Monocrystalline afterwards, it is (Fe that composition, which is made,0.83Ga0.17)99.95Tb0.05Magnetostriction materials (size Φ 7mm × 20mm).
After testing, should (Fe0.83Ga0.17)99.95Tb 0.05Tb elements are not dissolved into FeGa bases completely in magnetostriction materials
In body, but grain boundaries are pinned to separate out, and the material is<100>With<110>The polycrystalline material of orientation；In addition, should
(Fe0.83Ga0.17)99.95Tb 0.05The saturation magnetostriction constant of material is 300ppm or so, and the performance of material simultaneously is not apparent from carrying
It is high.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (6)
1. a kind of magnetostriction materials, it is characterised in that its composition is (Fe1-xGax)100-yREy, wherein 0.17≤x≤0.19,
The one or more of 0.01≤y≤0.2, RE in Tb, La, Sm, Dy, Lu, Ho, Er and Tm；
It is<100>The monocrystal material of orientation；
Saturation magnetic field is 100~500Oe, and saturation magnetostriction constant is up to 300~1500ppm.
2. magnetostriction materials according to claim 1, it is characterised in that its composition is (Fe0.83Ga0.17)99.95Tb0.05、
(Fe0.83Ga0.17)99.95Sm0.05、(Fe0.83Ga0.17)99.95Dy0.05、(Fe0.83Ga0.17)99.95Ho0.05、(Fe0.83Ga0.17)99.95Er0.05、(Fe0.83Ga0.17)99.95Tm0.05、(Fe0.81Ga0.19)99.95Tb0.05、(Fe0.81Ga0.19)99.95Sm0.05、
(Fe0.81Ga0.19)99.95Dy0.05、(Fe0.81Ga0.19)99.95Ho0.05、(Fe0.81Ga0.19)99.95Er0.05、(Fe0.81Ga0.19)99.95Tm0.05、(Fe0.83Ga0.17)99.97Lu0.03、(Fe0.81Ga0.19)99.96Dy0.04、(Fe0.82Ga0.18)99.98Sm0.02、
(Fe0.81Ga0.19)99.9Tm0.1、(Fe0.81Ga0.19)99.8La0.2、(Fe0.82Ga0.18)99.8(HoEr)0.2、(Fe0.83Ga0.17)99.84
(SmTm)0.16、(Fe0.82Ga0.18)99.85(HoErTm)0.15Or (Fe0.81Ga0.19)99.85(TbDyHo)0.15。
3. the preparation method of any magnetostriction materials of claim 1 to 2, it is characterised in that comprise the following steps：
1) Fe, Ga and RE raw material are equipped with according to the component requirements of magnetostriction materials；
2) Fe, Ga and RE raw material of outfit are smelted into mother alloy ingot；
3) mother alloy ingot is melted, and foundry alloy rod is made by suction pouring；
4) by the foundry alloy rod and<100>The FeGa single crystal seeds of orientation are placed in apparatus for directional solidification, and make FeGa monocrystalline
Coolant is immersed in seed crystal bottom, and after being vacuumized to apparatus for directional solidification and being filled with protective gas, heating makes foundry alloy rod completely molten
Melt and FeGa single crystal seeds top melts, the material of melting is carried out along FeGa single crystal seeds bottom pull into coolant
Directional solidification, and control the directional solidification thermograde be 1 × 105~9 × 105K/m, the speed of growth be 1000~
20000mm/h, the magnetostriction materials are made；
In step 4), the foundry alloy rod and FeGa single crystal seeds top are placed in the inside of hollow graphite calandria, pass through sense
Graphite heating body described in coil heats is answered, so that the melting completely of foundry alloy rod and the melting of FeGa single crystal seeds top；
In step 4), the heating includes implementing following operation at least once：
Graphite heating body is heated to 1550~1700 DEG C with 30~40 DEG C/min programming rate, treats that foundry alloy rod and FeGa are mono-
5~15min is incubated after the melting of grain of crystallization crystalline substance top, is then cooled to graphite heating body with 20~30 DEG C/min cooling rate
1450~1550 DEG C and 3~8min is incubated, then graphite heating body is heated to 1550 with 30~40 DEG C/min programming rate~
1700 DEG C and 5~15min of insulation；
In step 4), make FeGa single crystal seeds bottom immersion coolant and lower end in contact water-cooled metal part, the coolant are
Ga-In alloys.
4. preparation method according to claim 3, it is characterised in that in step 4), vacuumized simultaneously to apparatus for directional solidification
Being filled with protective gas includes implementing following operation at least once：
1.0 × 10 are evacuated to apparatus for directional solidification-3~5.0 × 10-3Protective gas is filled with after Pa, is treated in apparatus for directional solidification
Vacuum rise to 1.0 × 10-1~5 × 10-1Stop inflation after Pa.
5. according to any described preparation method of claim 3 to 4, it is characterised in that step 2) includes：
Fe, Ga and RE raw material of outfit are placed in smelting equipment, 5.0 × 10 are evacuated to smelting equipment-2~5.0 × 10- 3Protective gas is filled with after Pa, treats that the vacuum in smelting equipment rises to 1.0 × 10-1~5.0 × 10-1Stop inflation after Pa, it is real
After applying aforesaid operations at least once, under conditions of melting electric current is 100~150A melting raw material once more than, control molten every time
The time of refining is 3~5 minutes, and mother alloy ingot is made.
6. according to any described preparation method of claim 3 to 4, it is characterised in that step 3) includes：
The mother alloy ingot is placed in smelting equipment, 1.0 × 10 are evacuated to smelting equipment-3~5.0 × 10-3Filled after Pa
Enter protective gas, treat that the vacuum in smelting equipment rises to 1.0 × 10-1~5.0 × 10-1Stop inflation after Pa, in melting electricity
Flow for the mother alloy ingot is fused into aluminium alloy under conditions of 100~300A, and aluminium alloy is inhaled into casting and is made into mould
Foundry alloy rod.
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| JP2020050920A (en) * | 2018-09-27 | 2020-04-02 | パナソニックＩｐマネジメント株式会社 | Magnetostriction element and manufacturing method of magnetostriction element |
| JP7318884B2 (en) * | 2019-06-12 | 2023-08-01 | 住友金属鉱山株式会社 | Single crystal growth method for iron-gallium alloy |
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