CN102569638B - Adhesive giant magnetostrictive material with laminated structure height (111) orientation and preparation method thereof - Google Patents
Adhesive giant magnetostrictive material with laminated structure height (111) orientation and preparation method thereof Download PDFInfo
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- CN102569638B CN102569638B CN 201210034284 CN201210034284A CN102569638B CN 102569638 B CN102569638 B CN 102569638B CN 201210034284 CN201210034284 CN 201210034284 CN 201210034284 A CN201210034284 A CN 201210034284A CN 102569638 B CN102569638 B CN 102569638B
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- 239000000463 material Substances 0.000 title claims abstract description 221
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000853 adhesive Substances 0.000 title abstract description 8
- 230000001070 adhesive effect Effects 0.000 title abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 230000003068 static effect Effects 0.000 claims abstract description 17
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 38
- 238000002844 melting Methods 0.000 claims description 36
- 230000008018 melting Effects 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 19
- 239000003822 epoxy resin Substances 0.000 claims description 17
- 229920000647 polyepoxide Polymers 0.000 claims description 17
- 238000012360 testing method Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 14
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- 238000005303 weighing Methods 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 12
- 238000009434 installation Methods 0.000 claims description 12
- 230000010355 oscillation Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 8
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
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- -1 alkane diamines Chemical class 0.000 claims description 4
- 229960001124 trientine Drugs 0.000 claims description 4
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Abstract
The invention discloses an adhesive giant magnetostrictive material with laminated structure height (111) orientation and high-resistance low-loss characteristics and a preparation method thereof. Magnetocrystalline anisotropy of an alloy is controlled, and the component of the alloy is designed to be TbxDy1-xFey, wherein x is more than 0.4 and is less than and equal to 1, and y is more than or equal to 1.9 and is less than and equal to 1.95. The method comprises the following steps of: mixing alloy particles with the particle size of 10 to 300mu m, an adhesive, a curing agent and a process control agent, and performing dynamic magnetic field orientation under induction of a magnetic field with the intensity of 6,000 to 12,000Oe at the dynamic magnetic field frequency of 0.5 to 10Hz; and curing and molding in a water bath at the temperature of between 40 and 60 DEG C under a static magnetic field, and thus obtaining the adhesive giant magnetostrictive material with the laminated structure height (111) preferred orientation and high magnetoelastic strain of 1,900ppm.
Description
Technical field
The present invention relates to a kind of Tb-Dy-Fe magnetostrictive material, more particularly say, refer to a kind of layer structure that has, highly＜111 the Tb of orientation bonding
xDy
1-xFe
y(0.4＜x≤1,1.9≤y≤1.95) giant magnetostriction material and preparation method thereof.
Background technology
The giant magnetostriction material that with the TbDyFe alloy is representative has advantages such as the magnetostrictive strain amount is big, Curie temperature is high, electromechanical coupling factor is big, response speed is fast at high-power underwater communication because of it, and fields such as Precision Machining and Aero-Space have broad application prospects.Outside add the huge eddy current effect that high frequency action of alternating magnetic field under produce and improve its mechanical property in order to solve the TbDyFe alloy 20 end of the centurys, and bonding TbDyFe giant magnetostrictive driver composite material gets more and more people's extensive concerning.This composite material is to be mixed according to certain proportioning by TbDyFe alloying pellet and high polymer coupling agent.The high polymer coupling agent plays the effect of cutting off vortex flow between particle on the one hand, also reduces the magnetostriction performance of material simultaneously.Improving the degree of orientation of particle and obtaining more excellent distribution of particles tissue is to improve its magnetostrictive key.
Because the magnetostriction performance of giant magnetostrictive driver TbDyFe alloy has strong anisotropy, learn direction along different crystal and differ greatly λ
111＞＞λ
100,＜111〉oriented material best performances.Therefore can expect, with＜111 orientation TbDyFe single crystal grain is that functive prepares binding material, can obtain optimum magnetostriction performance.Yet existing report obtains height＜111 as yet〉the high-performance bonding giant magnetostriction material of orientation.
According to existing report, its reason mainly contains following 2 points.The TbDyFe foundry alloy that first part Study person adopts is＜112〉orientation.The Carman research group of the U.S. cuts into the needle-like short fiber with＜112〉orientation TbDyFe alloy bar materials, utilize its shape anisotropy under magnetic field, be orientated and prepare to have＜112〉the bonding giant magnetostriction material that is orientated.Its magnetostriction can reach 1600ppm, however its complex process, and cost is higher.The resin of Korea S scholar invention incorporates technology, oriented growth is combined with chemolysis, by inciting somebody to action rich rare earth pseudoeutectic phase and the SiO in＜112〉oriented crystal
2Reaction removes rich rare earth phase, infiltrates resin in the position, space that it stays then, make＜112〉orientation giant magnetostriction materials, but the magneto-strain maximum of its report only is 1013ppm.It two is because the magnetocrystalline anisotropy of TbDyFe foundry alloy is less.Studies show that, apply the degree of orientation that a static magnetic field can change particle at the batch mixing solidification process, is that alloying pellet has higher magnetocrystalline anisotropy yet particle overcomes the prerequisite that the viscous resistance of high polymer rotates under magnetic field effect.
Use Tb is disclosed in number of patent application CN200810073443.8
xDy
1-xFe
2-yAlloyed powder ring shaped agglutinate rare earth ultra-magnetostriction material processed; Use Tb is disclosed in number of patent application CN200610011895.4
1-xDy
xFe
2-yAlloyed powder agglutinate rare earth ultra-magnetostriction material processed; Alloying component Tb content x value is 0.2～0.4(atomic ratio in these two parts of patent applications) between.At this moment, because the magnetocrystalline anisotropy of alloying pellet is less, particle is finished orientation process by particle rotation in conjunction with the magnetic domain rotation under the effect that adds static magnetic field.Therefore particle＜111〉easy magnetizing axis can't rotate fully to outer magnetic field direction, cause the degree of orientation of particle not high.The magnetic field that applies in the orientation of particles process is static magnetic field, particle is trending towards forming approximate catenation under the situation of the original position of maintenance under the effect in magnetic field, thisly alignedly can't change the overall distribution of particle in polymer matrix, therefore the magnetostriction of particle generation passes to polymer matrix with some, and the magnetostriction that can't make adjacent particle produce is effectively transmitted.
Summary of the invention
The objective of the invention is to propose a kind of magnetocrystalline anisotropy by the regulation and control alloy, adopt the powder bonding, dynamically the high-intensity magnetic field induced orientation obtains to have layer structure, high resistance, large magneto-strain have height＜111 method of the anisotropic bond giant magnetostriction material of orientation.
Tb of the present invention
xDy
1-xFe
yThe alloying component of giant magnetostriction material is Tb
xDy
1-xFe
y, 0.4≤x≤1,1.9≤y≤1.95.
Prepare Tb of the present invention
xDy
1-xFe
yGiant magnetostriction material includes the following step:
The first step: preparation Tb
xDy
1-xFe
yAlloyed powder
The 1-1 step: press Tb
xDy
1-xFe
y, 0.4＜x≤1,1.9≤y≤1.95 target components take by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element are not less than 99.9%;
1-2 step: the melting raw material is put into vacuum arc furnace ignition carry out melting and make first materials;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1250 ℃～1350 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 20 ℃～40 ℃ with vacuum arc furnace ignition, takes out, and obtains first materials;
1-3 step: first materials are put into vacuum heat treatment furnace heat-treat and make second materials;
Heat-treat condition:
The vacuum degree of vacuum heat treatment furnace is less than 2 * 10
-3Pa;
Heat treatment temperature is 900 ℃～1000 ℃, heat treatment 4～12 hours, and be to carry out homogenization of composition under 99.99% the argon shield atmosphere in mass percent purity, be cooled to 20 ℃～40 ℃ with vacuum heat treatment furnace, take out, make second materials;
1-4 step: be brokenly under 99.99% the argon shield to make the Tb that particle diameter is 10～300 μ m in mass percent purity with second materials
xDy
1-xFe
yAlloyed powder;
Second step: preparation Tb
xDy
1-xFe
yCompound
The 2-1 step: the Tb of 100g processed
xDy
1-xFe
yCompound takes by weighing the Tb of 65～90g
xDy
1-xFe
yThe process control agent of the binding agent of alloyed powder, 9～28g, the curing agent of 2～6g, 0.05～1g;
Described binding agent selects for use Beijing Bo Lide commerce and trade Co., Ltd to produce epoxy resin E44, epoxy resin E51, epoxy resin 6101;
Described curing agent is selected triethylene tetramine, Meng alkane diamines, m-phenylene diamine (MPD) for use;
Described process control agent is selected methyl alcohol, propyl alcohol, pentane for use;
The 2-2 step: with Tb
xDy
1-xFe
yCompound mixes in acetone soln, and is stirring degassing under 30 ℃～50 ℃ conditions in temperature, stirs all to volatilize until acetone, makes the 3rd materials;
The 3rd step: sound attitude magnetic field orientating Tb processed
xDy
1-xFe
yMagnetostrictive material
The 3-1 step: in the 3rd materials injected plastic mould, both mold ends uses rubber stopper seal to form the first band material mould; Then the first band material mould is installed in the electromagnet, and the parallel installation with magnetic field line of longitudinal centre line of the first band material mould;
Rubber stopper remains on 0.1～0.5MPa to the pressure of the 3rd materials;
The 3-2 step: the dynamic magnetic field orientation is under the condition of 6000～12000Oe in central magnetic field intensity, and after 30～300 seconds, static 1～2 hour, taking-up made the second band material mould to the first band material mould around the O spot wobble;
The first band material mould around O point upwards the longitudinal centre line of pendulum be designated as first band around O point to the angle between the longitudinal centre line of the bottom with the first band material mould and expect mould angle of oscillation β, described first is with and expects that mould angle of oscillation β is 10 °～90 °;
The hunting frequency that the first band material mould is ordered around O is 0.5Hz～10Hz;
The 3-3 step: second water bath of being with the material mould to put into 40 ℃～80 ℃ is formed the 3rd band material mould; Then the 3rd band material mould is installed in the electromagnet, and the parallel installation with magnetic field line of longitudinal centre line of the 3rd band material mould;
The 3-4 step: the static magnetic field orientation is solidified, and is under the condition of 6000～12000Oe in central magnetic field intensity, handles through 2～4 hours resin solidifications, takes out, and obtains the Tb that bonds
xDy
1-xFe
yMagnetostrictive material.
Advantage of the present invention: this material will be by having the Tb of magnetostrictive effect
xDy
1-xFe
y(atomic ratio is 0.4＜x≤1,1.9≤y≤1.95) particle mixes with high-resistance epoxy resin, earlier induces orientation down at dynamic high-intensity magnetic field, induces curing molding down at static high-intensity magnetic field then, makes Tb
xDy
1-xFe
yParticle is arranged and the formation layer structure along magnetic line of force direction, and the Tb in every layer
xDy
1-xFe
yParticle is catenation, make each the layer in Tb
xDy
1-xFe
yThe magnetostriction of particle can effectively pass to adjacent particle.Simultaneously because particle has higher magnetocrystalline anisotropy energy, and particle rotates in the magnetic field orientating process, and its easy axis direction is parallel with magnetic direction, make the bonding giant magnetostriction material have highly＜111〉be orientated and have a significant pressure effect characteristic.。
The bonding Tb that the present invention makes
xDy
1-xFe
y(atomic ratio is 0.4＜x≤1,1.9≤y≤1.95) giant magnetostriction material has highly＜111〉preferred orientation.Its resistivity is 1.23 Ω m～8.00 Ω m.The test magnetic field be 0～7600Oe, test pressure is 0～24MPa, maximum magneto-strain is 1600ppm～1900ppm.At high frequency 1 * 10
5Eddy current loss value under the Hz is 510W/m
3～570W/m
3
Description of drawings
Fig. 1 expects that with first band mould is installed in the position view in the electromagnet.
Fig. 2 swings the position view that is installed in the electromagnet with the second band material mould.
Fig. 3 expects that with the 3rd band mould is installed in the position view in the electromagnet.
Fig. 4 A is the bonding Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95The X-ray diffractogram of giant magnetostriction material.
Fig. 4 B is the bonding Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95The magneto-strain of giant magnetostriction material and magnetic field dependence figure.
Fig. 4 C is the bonding Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95The eddy current loss of giant magnetostriction material and frequency relation figure.
Fig. 4 D is the bonding Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95The optics metallurgical figure of giant magnetostriction material.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Make and have layer structure, highly＜111 orientation bonding Tb
xDy
1-xFe
y(atomic ratio is 0.4＜x≤1,1.9≤y≤1.95) giant magnetostriction material, its preparation technology comprises the following steps:
The first step: preparation Tb
xDy
1-xFe
yAlloyed powder
The 1-1 step: press Tb
xDy
1-xFe
y(0.4＜x≤1,1.9≤y≤1.95) target component takes by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element is not less than 99.9%;
1-2 step: the melting raw material is put into vacuum arc furnace ignition carry out melting and make first materials;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1250 ℃～1350 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 20 ℃～40 ℃ with vacuum arc furnace ignition, takes out, and obtains first materials;
1-3 step: first materials are put into vacuum heat treatment furnace heat-treat and make second materials;
Heat-treat condition:
The vacuum degree of vacuum heat treatment furnace is less than 2 * 10
-3Pa;
Heat treatment temperature is 900 ℃～1000 ℃, heat treatment 4～12 hours, and be to carry out homogenization of composition under 99.99% the argon shield atmosphere in mass percent purity, be cooled to 20 ℃～40 ℃ with vacuum heat treatment furnace, take out, make second materials;
1-4 step: be brokenly under 99.99% the argon shield to make the Tb that particle diameter is 10～300 μ m in mass percent purity with second materials
xDy
1-xFe
yAlloyed powder;
Second step: preparation Tb
xDy
1-xFe
yCompound
The 2-1 step: the Tb of 100g processed
xDy
1-xFe
yCompound takes by weighing the Tb of 65～90g
xDy
1-xFe
yThe process control agent of the binding agent of alloyed powder, 9～28g, the curing agent of 2～6g, 0.05～1g;
Described binding agent selects for use Beijing Bo Lide commerce and trade Co., Ltd to produce epoxy resin E44, epoxy resin E51, epoxy resin 6101;
Described curing agent is selected triethylene tetramine, Meng alkane diamines, m-phenylene diamine (MPD) for use;
Described process control agent is selected methyl alcohol, propyl alcohol, pentane for use;
The 2-2 step: with Tb
xDy
1-xFe
yCompound mixes in acetone soln, and is stirring degassing under 30 ℃～50 ℃ conditions in temperature, stirs all to volatilize until acetone, makes the 3rd materials;
The 3rd step: sound attitude magnetic field orientating Tb processed
xDy
1-xFe
yMagnetostrictive material
The 3-1 step: in the 3rd materials injected plastic mould, both mold ends uses rubber stopper seal to form the first band material mould; Referring to shown in Figure 1 the first band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the first band material mould;
Rubber stopper remains on 0.1～0.5MPa to the pressure of the 3rd materials;
In the present invention, longitudinal centre line and the longitudinal center line of the first band material mould intersect at the O point;
The 3-2 step: the dynamic magnetic field orientation is under the condition of 6000～12000Oe in central magnetic field intensity, and after 30～300 seconds, static 1～2 hour, taking-up made the second band material mould to the first band material mould around the O spot wobble;
Referring to shown in Figure 2, the first band material mould around O point upwards the longitudinal centre line of pendulum be designated as first band around O point to the angle between the longitudinal centre line of the bottom with the first band material mould and expect mould angle of oscillation β, described first is with and expects that mould angle of oscillation β is 10 °～90 °;
The hunting frequency that the first band material mould is ordered around O is 0.5Hz～10Hz;
The 3-3 step: second water bath of being with the material mould to put into 40 ℃～80 ℃ is formed the 3rd band material mould; Referring to shown in Figure 3 the 3rd band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the 3rd band material mould;
The 3-4 step: the static magnetic field orientation is solidified, and is under the condition of 6000～12000Oe in central magnetic field intensity, handles through 2～4 hours resin solidifications, takes out, and obtains the Tb that bonds
xDy
1-xFe
yMagnetostrictive material.
In the present invention, the bonding Tb that makes
xDy
1-xFe
yMagnetostrictive material have height＜111〉preferred orientation, and Tb simultaneously bonds
xDy
1-xFe
yTb in the magnetostrictive material
xDy
1-xFe
yIt is that layer structure is arranged that particle presents in resin matrix along the alignment magnetic field direction, and every layer of Tb
xDy
1-xFe
yParticle is catenation.
Embodiment 1 system bonding Tb
0.5Dy
0.5Fe
1.95Giant magnetostriction material
The first step: preparation Tb
0.5Dy
0.5Fe
1.95Alloyed powder
The 1-1 step: press Tb
0.5Dy
0.5Fe
1.95Target component takes by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element is not less than 99.9%;
1-2 step: the melting raw material is put into vacuum arc furnace ignition carry out melting and make first materials;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1300 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 25 ℃ with vacuum arc furnace ignition, takes out, and obtains first materials;
1-3 step: first materials are put into vacuum heat treatment furnace heat-treat and make second materials;
Heat-treat condition:
The vacuum degree of vacuum heat treatment furnace is less than 2 * 10
-3Pa;
Heat treatment temperature is 1000 ℃, heat treatment 6 hours, and be to carry out homogenization of composition under 99.99% the argon shield atmosphere in mass percent purity, be cooled to 25 ℃ with vacuum heat treatment furnace, take out, make second materials;
1-4 step: be brokenly under 99.99% the argon shield to make the Tb that average grain diameter is 250 μ m in mass percent purity with second materials
0.5Dy
0.5Fe
1.95Alloyed powder;
Second step: preparation Tb
0.5Dy
0.5Fe
1.95Compound
The 2-1 step: the Tb of 100g processed
0.5Dy
0.5Fe
1.95Compound takes by weighing the Tb of 80g
0.5Dy
0.5Fe
1.95The process control agent of the binding agent of alloyed powder, 13g, the curing agent of 6g, 1g;
Described binding agent selects for use Beijing Bo Lide commerce and trade Co., Ltd to produce epoxy resin E44;
Described curing agent is selected triethylene tetramine for use;
Described process control agent is selected methyl alcohol for use;
The 2-2 step: with Tb
0.5Dy
0.5Fe
1.95Compound mixes in acetone soln, and is stirring degassing under 30 ℃ of conditions in temperature, stirs all to volatilize until acetone, makes the 3rd materials;
The 3rd step: sound attitude magnetic field orientating Tb processed
0.5Dy
0.5Fe
1.95Magnetostrictive material
The 3-1 step: in the 3rd materials injected plastic mould, both mold ends uses rubber stopper seal to form the first band material mould; Referring to shown in Figure 1 the first band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the first band material mould;
Rubber stopper remains on 0.2MPa to the pressure of the 3rd materials;
In the present invention, longitudinal centre line and the longitudinal center line of the first band material mould intersect at the O point;
The 3-2 step: the dynamic magnetic field orientation is under the condition of 8000Oe in central magnetic field intensity, and after 300 seconds, static 2 hours, taking-up made the second band material mould to the first band material mould around the O spot wobble;
Referring to shown in Figure 2, the first band material mould around O point upwards the longitudinal centre line of pendulum be designated as first band around O point to the angle between the longitudinal centre line of the bottom with the first band material mould and expect mould angle of oscillation β, described first is with and expects that mould angle of oscillation β is 45 °;
The hunting frequency that the first band material mould is ordered around O is 1Hz;
The 3-3 step: second water bath of being with the material mould to put into 50 ℃ is formed the 3rd band material mould; Referring to shown in Figure 3 the 3rd band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the 3rd band material mould;
The 3-4 step: the static magnetic field orientation is solidified, and is under the condition of 8000Oe in central magnetic field intensity, handles through 2 hours resin solidifications, takes out, and obtains Tb
0.5Dy
0.5Fe
1.95Magnetostrictive material.
In the present invention, the Tb that makes
0.5Dy
0.5Fe
1.95Magnetostrictive material have height＜111〉preferred orientation, simultaneously Tb
0.5Dy
0.5Fe
1.95Tb in the magnetostrictive material
0.5Dy
0.5Fe
1.95It is that layer structure is arranged that particle presents in resin matrix along the alignment magnetic field direction.
Adopt Japanese D/Max2200PC type X-ray diffractometer of science to carry out X-ray diffraction analysis, the result is (ordinate is represented relative intensity, and abscissa is represented 2 θ angles) shown in Fig. 4 A.Tb
0.5Dy
0.5Fe
1.95Particle has height＜111〉preferred orientation under induced by magnetic field.
Employing standard four contact resistance strain gauge methods carry out the magneto-strain test, and test magnetic field is 0～7600Oe, and test pressure is 0MPa, 3MPa, 9MPa, 24MPa, and test result is (ordinate is represented magnetostriction, the abscissa magnetic field intensity) shown in Fig. 4 B.Be 1720ppm when being 1611ppm, 24MPa when being 1419ppm, 9MPa when being 1160ppm, 3MPa during the magnetostriction coefficient 0MPa of anisotropic bond material.The Tb that this explanation embodiment 1 makes
0.5Dy
0.5Fe
1.95Magnetostrictive material have significant pressure effect.
Epoxide resin conductive adhesive evenly is coated on the Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95On the magnetostrictive material surface, and make two electrodes, use universal instrument to measure the Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95The resistance of magnetostrictive material, resistivity are 1.23 Ω m.
Comparative Examples vacuum melting Tb
0.5Dy
0.5Fe
1.95Bar
Press Tb
0.5Dy
0.5Fe
1.95Target component takes by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element is not less than 99.9%; The melting raw material is put into vacuum arc furnace ignition to carry out melting and makes Tb
0.5Dy
0.5Fe
1.95Bar;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1300 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 25 ℃ with vacuum arc furnace ignition, takes out, and obtains Tb
0.5Dy
0.5Fe
1.95Bar.
Epoxide resin conductive adhesive evenly is coated on Tb
0.5Dy
0.5Fe
1.95On the bar surface, and make two electrodes, use universal instrument to measure Tb
0.5Dy
0.5Fe
1.95The resistance of bar, resistivity are 0.5 * 10
-6Ω m.
The Tb that comparative example 1 makes
0.5Dy
0.5Fe
1.95The Tb that magnetostrictive material and Comparative Examples make
0.5Dy
0.5Fe
1.95The resistivity of bar, the Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95Magnetostrictive material resistivity improves 6 orders of magnitude.
Adopt TPS-500M soft magnetic material measuring instrument to come the eddy current loss performance of exosyndrome material: to record the Tb that embodiment 1 makes
0.5Dy
0.5Fe
1.95The eddy current loss value of magnetostrictive material is 570W/m
3, shown in Fig. 4 C (ordinate is represented the eddy current loss value, and abscissa is represented frequency).The Tb that Comparative Examples makes
0.5Dy
0.5Fe
1.95The eddy current loss value of bar is 15405W/m
3, shown in Fig. 4 C.Through contrasting at high frequency 1 * 10
5Eddy current loss value under the Hz only is Tb
0.5Dy
0.5Fe
1.953.7% of bar.
The bonding Tb that adopts BM51X metallography microscope sem observation embodiment 1 to make
0.5Dy
0.5Fe
1.95The metallographic microstructure of magnetostrictive material.The bonding Tb that embodiment 1 is made
0.5Dy
0.5Fe
1.95The cross section of magnetostrictive material (being bar) uses abrasive paper for metallograph polishing and polishing, and at the metallographic microstructure of BM51X metallography microscope sem observation material, the result is shown in Fig. 4 D.Bonding Tb
0.5Dy
0.5Fe
1.95Tb in the magnetostrictive material
0.5Dy
0.5Fe
1.95Particle is arranged along magnetic line of force direction under induced by magnetic field, the visible Tb of microscopic structure
0.5Dy
0.5Fe
1.95Particle is layer structure in epoxy resin-base arranges, and every layer of Tb
0.5Dy
0.5Fe
1.95Particle is catenation.
The first step: preparation Tb
0.95Dy
0.05Fe
1.9Alloyed powder
The 1-1 step: press Tb
0.95Dy
0.05Fe
1.9Target component takes by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element is not less than 99.9%;
1-2 step: the melting raw material is put into vacuum arc furnace ignition carry out melting and make first materials;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1250 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 40 ℃ with vacuum arc furnace ignition, takes out, and obtains first materials;
1-3 step: first materials are put into vacuum heat treatment furnace heat-treat and make second materials;
Heat-treat condition:
The vacuum degree of vacuum heat treatment furnace is less than 2 * 10
-3Pa;
Heat treatment temperature is 900 ℃, heat treatment 12 hours, and be to carry out homogenization of composition under 99.99% the argon shield atmosphere in mass percent purity, be cooled to 40 ℃ with vacuum heat treatment furnace, take out, make second materials;
1-4 step: be brokenly under 99.99% the argon shield to make the Tb that average grain diameter is 50 μ m in mass percent purity with second materials
0.95Dy
0.05Fe
1.9Alloyed powder;
Second step: preparation Tb
0.95Dy
0.05Fe
1.9Compound
The 2-1 step: the Tb of 100g processed
0.95Dy
0.05Fe
1.9Compound takes by weighing the Tb of 67g
0.95Dy
0.05Fe
1.9The process control agent of the binding agent of alloyed powder, 28g, the curing agent of 4.95g, 0.05g;
The epoxy resin E51 that described binding agent selects for use Beijing Bo Lide commerce and trade Co., Ltd to produce;
Described curing agent is selected m-phenylene diamine (MPD) for use;
Described process control agent is selected pentane for use;
The 2-2 step: with Tb
0.95Dy
0.05Fe
1.9Compound mixes in acetone soln, and is stirring degassing under 50 ℃ of conditions in temperature, stirs all to volatilize until acetone, makes the 3rd materials;
The 3rd step: sound attitude magnetic field orientating Tb processed
0.95Dy
0.05Fe
1.9Magnetostrictive material
The 3-1 step: in the 3rd materials injected plastic mould, both mold ends uses rubber stopper seal to form the first band material mould; Referring to shown in Figure 1 the first band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the first band material mould;
Rubber stopper remains on 0.5MPa to the pressure of the 3rd materials;
In the present invention, longitudinal centre line and the longitudinal center line of the first band material mould intersect at the O point;
The 3-2 step: the dynamic magnetic field orientation is under the condition of 6000Oe in central magnetic field intensity, and after 100 seconds, static 1 hour, taking-up made the second band material mould to the first band material mould around the O spot wobble;
Referring to shown in Figure 2, the first band material mould around O point upwards the longitudinal centre line of pendulum be designated as first band around O point to the angle between the longitudinal centre line of the bottom with the first band material mould and expect mould angle of oscillation β, described first is with and expects that mould angle of oscillation β is 10 °;
The hunting frequency that the first band material mould is ordered around O is 9Hz;
The 3-3 step: second water bath of being with the material mould to put into 70 ℃ is formed the 3rd band material mould; Referring to shown in Figure 3 the 3rd band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the 3rd band material mould;
The 3-4 step: the static magnetic field orientation is solidified, and is under the condition of 6000Oe in central magnetic field intensity, handles through 4 hours resin solidifications, takes out, and obtains the Tb that bonds
0.95Dy
0.05Fe
1.9Magnetostrictive material.
Adopt Japanese D/Max2200PC type X-ray diffractometer of science to carry out X-ray diffraction analysis, Tb
0.95Dy
0.05Fe
1.9Particle has height＜111〉preferred orientation under induced by magnetic field.
Employing standard four contact resistance strain gauge methods carry out the magneto-strain test, test magnetic field is 0～7600Oe, test pressure is 0MPa, 3MPa, 9MPa, 24MPa, the 1900ppm the when magnetostriction coefficient of anisotropic bond material is 1710ppm, 24MPa when being 1490ppm, 9MPa when being 1130ppm, 3MPa during by 0MPa.The bonding Tb that this explanation embodiment 2 makes
0.95Dy
0.05Fe
1.9Magnetostrictive material have significant pressure effect.
Epoxide resin conductive adhesive evenly is coated on the bonding Tb that embodiment 2 makes
0.95Dy
0.05Fe
1.9On the magnetostrictive material surface, and make two electrodes, use universal instrument to measure the bonding Tb that embodiment 2 makes
0.95Dy
0.05Fe
1.9The resistance of magnetostrictive material, resistivity are 8.00 Ω m.
Adopt TPS-500M soft magnetic material measuring instrument to come the eddy current loss performance of exosyndrome material: to record the bonding Tb that embodiment 2 makes
0.95Dy
0.05Fe
1.9The eddy current loss value of magnetostrictive material is 534W/m
3
The first step: preparation Tb
0.7Dy
0.3Fe
1.93Alloyed powder
The 1-1 step: press Tb
0.7Dy
0.3Fe
1.93Target component takes by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element is not less than 99.9%;
1-2 step: the melting raw material is put into vacuum arc furnace ignition carry out melting and make first materials;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1350 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 30 ℃ with vacuum arc furnace ignition, takes out, and obtains first materials;
1-3 step: first materials are put into vacuum heat treatment furnace heat-treat and make second materials;
Heat-treat condition:
The vacuum degree of vacuum heat treatment furnace is less than 2 * 10
-3Pa;
Heat treatment temperature is 950 ℃, heat treatment 8 hours, and be to carry out homogenization of composition under 99.99% the argon shield atmosphere in mass percent purity, be cooled to 30 ℃ with vacuum heat treatment furnace, take out, make second materials;
1-4 step: be brokenly under 99.99% the argon shield to make the Tb that average grain diameter is 150 μ m in mass percent purity with second materials
0.7Dy
0.3Fe
1.93Alloyed powder;
Second step: preparation Tb
0.7Dy
0.3Fe
1.93Compound
The 2-1 step: the Tb of 100g processed
0.7Dy
0.3Fe
1.93Compound takes by weighing the Tb of 88g
0.7Dy
0.3Fe
1.93The process control agent of the binding agent of alloyed powder, 9g, the curing agent of 2g, 1g;
The epoxy resin 6101 that described binding agent selects for use Beijing Bo Lide commerce and trade Co., Ltd to produce;
Described curing agent is selected alkane diamines in the Meng for use;
Described process control agent is selected propyl alcohol for use;
The 2-2 step: with Tb
0.7Dy
0.3Fe
1.93Compound mixes in acetone soln, and is stirring degassing under 40 ℃ of conditions in temperature, stirs all to volatilize until acetone, makes the 3rd materials;
The 3rd step: sound attitude magnetic field orientating Tb processed
0.7Dy
0.3Fe
1.93Magnetostrictive material
The 3-1 step: in the 3rd materials injected plastic mould, both mold ends uses rubber stopper seal to form the first band material mould; Referring to shown in Figure 1 the first band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the first band material mould;
Rubber stopper remains on 0.3MPa to the pressure of the 3rd materials;
In the present invention, longitudinal centre line and the longitudinal center line of the first band material mould intersect at the O point;
The 3-2 step: the dynamic magnetic field orientation is under the condition of 12000Oe in central magnetic field intensity, and after 60 seconds, static 1.5 hours, taking-up made the second band material mould to the first band material mould around the O spot wobble;
Referring to shown in Figure 2, the first band material mould around O point upwards the longitudinal centre line of pendulum be designated as first band around O point to the angle between the longitudinal centre line of the bottom with the first band material mould and expect mould angle of oscillation β, described first is with and expects that mould angle of oscillation β is 60 °;
The hunting frequency that the first band material mould is ordered around O is 5Hz;
The 3-3 step: second water bath of being with the material mould to put into 40 ℃ is formed the 3rd band material mould; Referring to shown in Figure 3 the 3rd band material mould is installed in the electromagnet then, and the parallel installation with magnetic field line of longitudinal centre line of the 3rd band material mould;
The 3-4 step: the static magnetic field orientation is solidified, and is under the condition of 12000Oe in central magnetic field intensity, handles through 3 hours resin solidifications, takes out, and obtains the Tb that bonds
0.7Dy
0.3Fe
1.93Magnetostrictive material.
Adopt Japanese D/Max2200PC type X-ray diffractometer of science to carry out X-ray diffraction analysis, Tb
0.7Dy
0.3Fe
1.93Particle has height＜111〉preferred orientation under induced by magnetic field.
Employing standard four contact resistance strain gauge methods carry out the magneto-strain test, test magnetic field is 0～7600Oe, test pressure is 0MPa, 3MPa, 9MPa, 24MPa, the 1770ppm the when magnetostriction coefficient of anisotropic bond material is 1670ppm, 24MPa when being 1460ppm, 9MPa when being 1175ppm, 3MPa during by 0MPa.The bonding Tb that this explanation embodiment 3 makes
0.7Dy
0.3Fe
1.93Magnetostrictive material have significant pressure effect.
Epoxide resin conductive adhesive evenly is coated on the bonding Tb that embodiment 3 makes
0.7Dy
0.3Fe
1.93On the magnetostrictive material surface, and make two electrodes, use universal instrument to measure the bonding Tb that embodiment 3 makes
0.7Dy
0.3Fe
1.93The resistance of magnetostrictive material, resistivity are 5.06 Ω m.
Adopt TPS-500M soft magnetic material measuring instrument to come the eddy current loss performance of exosyndrome material: to record the bonding Tb that embodiment 3 makes
0.7Dy
0.3Fe
1.93The eddy current loss value of magnetostrictive material is 510W/m
3
Claims (10)
1. one kind has layer structure height＜111〉orientation bonding giant magnetostriction material, it is characterized in that: the alloying component of described bonding giant magnetostriction material is Tb
xDy
1-xFe
y, 0.4＜x≤1,1.9≤y≤1.95.
2. according to claim 1ly have layer structure height＜111〉orientation bonding giant magnetostriction material, it is characterized in that: Tb
xDy
1-xFe
yGiant magnetostriction material has height＜111〉preferred orientation.
3. according to claim 1ly have layer structure height＜111〉orientation bonding giant magnetostriction material, it is characterized in that: Tb
xDy
1-xFe
yThe resistivity of giant magnetostriction material is 1.23 Ω m～8.00 Ω m.
4. according to claim 1ly have layer structure height＜111〉orientation bonding giant magnetostriction material, it is characterized in that: Tb
xDy
1-xThe Fey giant magnetostriction material is 0～7600Oe in test magnetic field, and test pressure is 0～24MPa, and maximum magneto-strain is 1600ppm～1900ppm.
5. according to claim 1ly have layer structure height＜111〉orientation bonding giant magnetostriction material, it is characterized in that: Tb
xDy
1-xFe
yGiant magnetostriction material is at high frequency 1 * 10
5Eddy current loss value under the Hz is 510W/m
3～570W/m
3
6. prepare layer structure height＜111 that have as claimed in claim 1〉method of orientation bonding giant magnetostriction material, it is characterized in that including the following step:
The first step: preparation Tb
xDy
1-xFe
yAlloyed powder
The 1-1 step: press Tb
xDy
1-xFe
y, 0.4＜x≤1,1.9≤y≤1.95 target components take by weighing Tb, Dy, each element of Fe, mix to obtain the melting raw material, and the mass percent purity of each element are not less than 99.9%;
1-2 step: the melting raw material is put into vacuum arc furnace ignition carry out melting and make first materials;
Melting condition:
The vacuum degree of vacuum arc furnace ignition is less than 2 * 10
-3Pa;
Smelting temperature is 1250 ℃～1350 ℃, and is that melting is even under 99.99% the argon shield atmosphere in mass percent purity, is cooled to 20 ℃～40 ℃ with vacuum arc furnace ignition, takes out, and obtains first materials;
1-3 step: first materials are put into vacuum heat treatment furnace heat-treat and make second materials;
Heat-treat condition:
The vacuum degree of vacuum heat treatment furnace is less than 2 * 10
-3Pa;
Heat treatment temperature is 900 ℃～1000 ℃, heat treatment 4～12 hours, and be to carry out homogenization of composition under 99.99% the argon shield atmosphere in mass percent purity, be cooled to 20 ℃～40 ℃ with vacuum heat treatment furnace, take out, make second materials;
1-4 step: be brokenly under 99.99% the argon shield to make the Tb that particle diameter is 10～300 μ m in mass percent purity with second materials
xDy
1-xFe
yAlloyed powder;
Second step: preparation Tb
xDy
1-xFe
yCompound
The 2-1 step: the Tb of 100g processed
xDy
1-xFe
yCompound takes by weighing the Tb of 65～90g
xDy
1-xFe
yThe process control agent of the binding agent of alloyed powder, 9～28g, the curing agent of 2～6g, 0.05～1g;
Described binding agent selects for use Beijing Bo Lide commerce and trade Co., Ltd to produce epoxy resin E44, epoxy resin E51, epoxy resin 6101;
Described curing agent is selected triethylene tetramine, Meng alkane diamines, m-phenylene diamine (MPD) for use;
Described process control agent is selected methyl alcohol, propyl alcohol, pentane for use;
The 2-2 step: with Tb
xDy
1-xFe
yCompound mixes in acetone soln, and is stirring degassing under 30 ℃～50 ℃ conditions in temperature, stirs all to volatilize until acetone, makes the 3rd materials;
The 3rd step: sound attitude magnetic field orientating Tb processed
xDy
1-xFe
yMagnetostrictive material
The 3-1 step: in the 3rd materials injected plastic mould, both mold ends uses rubber stopper seal to form the first band material mould; Then the first band material mould is installed in the electromagnet, and the parallel installation with magnetic field line of longitudinal centre line of the first band material mould;
Rubber stopper remains on 0.1～0.5MPa to the pressure of the 3rd materials;
The 3-2 step: the dynamic magnetic field orientation is under the condition of 6000～12000Oe in central magnetic field intensity, and after 30～300 seconds, static 1～2 hour, taking-up made the second band material mould to the first band material mould around the O spot wobble;
The first band material mould around O point upwards the longitudinal centre line of pendulum be designated as first band around O point to the angle between the longitudinal centre line of the bottom with the first band material mould and expect mould angle of oscillation β, described first is with and expects that mould angle of oscillation β is 10 °～90 °;
The hunting frequency that the first band material mould is ordered around O is 0.5Hz～10Hz;
The 3-3 step: second water bath of being with the material mould to put into 40 ℃～80 ℃ is formed the 3rd band material mould; Then the 3rd band material mould is installed in the electromagnet, and the parallel installation with magnetic field line of longitudinal centre line of the 3rd band material mould;
The 3-4 step: the static magnetic field orientation is solidified, and is under the condition of 6000～12000Oe in central magnetic field intensity, handles through 2～4 hours resin solidifications, takes out, and obtains the Tb that bonds
xDy
1-xFe
yMagnetostrictive material.
7. preparation according to claim 6 has layer structure height＜111〉method of orientation bonding giant magnetostriction material, it is characterized in that: the bonding Tb that makes
xDy
1-xFe
yMagnetostrictive material have height＜111〉preferred orientation, simultaneously Tb
xDy
1-xFe
yTb in the magnetostrictive material
xDy
1-xFe
yIt is that layer structure is arranged that particle presents in resin matrix along the alignment magnetic field direction, and every layer of Tb
xDy
1-xFe
yParticle is catenation.
8. preparation according to claim 6 has layer structure height＜111〉method of orientation bonding giant magnetostriction material, it is characterized in that: the bonding Tb that makes
xDy
1-xFe
yThe resistivity of giant magnetostriction material is 1.23 Ω m～8.00 Ω m.
9. preparation according to claim 6 has layer structure height＜111〉method of orientation bonding giant magnetostriction material, it is characterized in that: the bonding Tb that makes
xDy
1-xFe
yGiant magnetostriction material is 0～7600Oe in test magnetic field, and test pressure is 0～24MPa, and maximum magneto-strain is 1600ppm～1900ppm.
10. preparation according to claim 6 has layer structure height＜111〉method of orientation bonding giant magnetostriction material, it is characterized in that: the bonding Tb that makes
xDy
1-xFe
yGiant magnetostriction material is at high frequency 1 * 10
5Eddy current loss value under the Hz is 510W/m
3～570W/m
3
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| CN109811163A (en) * | 2017-11-20 | 2019-05-28 | 有研稀土新材料股份有限公司 | A kind of preparation method of sintering rare-earth giant magnetostrictive material |
| CN111326303A (en) * | 2020-03-04 | 2020-06-23 | 南京大学 | Method for manufacturing rare earth alloy spherical single crystal magnetic powder and <111> oriented rare earth giant magnetostrictive material |
| CN113073249B (en) * | 2021-02-26 | 2022-12-02 | 湖南大学 | Preparation method of <111> + <110> preferred orientation giant magnetostrictive material TbxDy1-xFey |
| CN114002627B (en) * | 2021-10-29 | 2023-08-25 | 深圳技术大学 | Microcosmic in-situ measurement system of magnetostrictive material under strong magnetic field |
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| CN100524871C (en) * | 2007-08-27 | 2009-08-05 | 北京航空航天大学 | Wide-temperature range narrow hysteresis Ho series giant magnetostriction material and its oriented crystal and single crystal preparation method |
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