CN103647019A - Giant magnetostrictive material brewed via light rare earth and preparation technology of giant magnetostrictive material - Google Patents

Giant magnetostrictive material brewed via light rare earth and preparation technology of giant magnetostrictive material Download PDF

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CN103647019A
CN103647019A CN201310617774.4A CN201310617774A CN103647019A CN 103647019 A CN103647019 A CN 103647019A CN 201310617774 A CN201310617774 A CN 201310617774A CN 103647019 A CN103647019 A CN 103647019A
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rare earth
light rare
melting
alloy
magnetostrictive material
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CN103647019B (en
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时阳光
胡成超
阚彩侠
施大宁
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention provides a method for directly obtaining orientation columnar crystal giant magnetostrictive material by slightly adding light rare earth to a conventional compensation system and controlling a smelting process. Large intrinsic magnetostrictive and low magneto-crystalline anisotropic characteristics of light rare earth of Pr and Nd are utilized by the method to optimize the compensation system. Besides, a super-cooling program is additionally arranged in the smelting so that the rare earth giant magnetostrictive material with partial (100) or (111) orientation is directly obtained. The method is simple and easy to carry out and economical in time and energy consumption cost so that one approach is provided for rapidly preparing orientation crystal.

Description

A kind of giant magnetostriction material and preparation technology thereof of light rare earth modulation
Technical field:
The giant magnetostriction material and the preparation technology thereof that the present invention relates to a kind of light rare earth modulation, it belongs to metal material field.
Background technology:
Rare-Earth Giant Magnetostrictive Materials is the new function material of the exploitation eighties, mainly refers to RFe 2cube Laves phase compound between (R=rare earth) rare earth metal.This class material can be realized the efficient conversion between electromagnetic energy and mechanical energy.The O.D.McMasters cooperation of the A.E.Clark Deng Yu USDOE Ames Lab in weapon research center, USN surface, by the magnetocrystalline anisotropy between rare earth, compensate, obtained the Tb that not only there is low large magnetostriction but also there is low magnetocrystalline anisotropy 0.27dy 0.73fe 2alloy.It is the United States Patent (USP) of US3949351 and US4308474 that this invention has been applied as the patent No..At the end of the eighties, this counterfeit dualization alloy be take in the RTREMA company of famous American makes rare earth giant magnetostrictive material commercialization as basis, and its trade names are Terfenol-D.The preparation technology of traditional Rare-Earth Giant Magnetostrictive Materials is grasped by the U.S. mostly, if the patent No.s of 1986 are that US4609402, the patent No. of 1988 are that United States Patent (USP) that US4770704, the patent No. of 1989 are US4818304 has been announced respectively the method that vertical area fusion method, pulling method, magnetic-field annealing method etc. are prepared rare earth giant magnetostrictive material.Japanology person in 2002 utilizes and under microgravity condition, obtains <111> orientation TbDyFe alloy.China Patent Publication No. CN1232275A rare-earth-iron super magnetostriction material and manufacturing process provide a kind of <110> of preparation to be oriented to main manufacturing process.China Patent Publication No. CN1435851A giant magnetostriction material and manufacturing process provide a kind of <113> to be oriented to main giant magnetostriction material manufacturing process.Although the magnetostriction character of the material that directional solidification method obtains is significantly improved, but prepare directed alloy, need to first obtain alloy mother metal and then at crystal growing furnace, regrow and pilot process is long, can not be interrupted, the preparation cost of material be increased and consuming time longer.
Single ion model calculates and shows PrFe 2spontaneous magnetostriction coefficient lambda at absolute zero 111reach 5600ppm, compare TbFe 2(λ 111=4400ppm) and DyFe 2(λ 111=4200ppm) there is higher theoretical magnetostriction value.And NdFe 2the magnetostriction coefficient of absolute zero is also being reached to 2000ppm, comparing HoFe 2(λ 111=1600ppm) large 25%.In addition, the resource of light rare earth Pr, Nd is abundanter, than the low price of heavy rare earth.So the exploitation of light rare earth magnetostrictive material is devoted in much work, the method that as open in Chinese patent CN1096546, CN1125265, CN1232275, CN1435851 etc. all take part to replace is added Pr in the counterfeit dualization alloy of TbDyFe base, is intended to obtain the new material of high Pr content high-magnetostriction.But excessive light rare earth adds the generation that membership causes second-phase, have a strong impact on the magnetostriction character of material.We find in the development process of light rare earth giant magnetostriction material, and the introducing of appropriate light rare earth Pr, Nd can effectively reduce the magnetocrystalline anisotropy of TbDyFe base magnetic striction material.In addition, we can directly obtain partially oriented magnetostrictive material by controlling fusion process, make like this preparation cost of material when keeping the excellent Magnetostriction of material also greatly reduce.
Summary of the invention:
The invention provides a kind of giant magnetostriction material and preparation technology thereof of light rare earth modulation.Adopt light rare earth base bucking-out system trace to substitute traditional rare earth bucking-out system and control fusion process and directly obtain the brilliant giant magnetostriction material of columnar orientation.
The present invention adopts following technical scheme: a kind of giant magnetostriction material of light rare earth modulation, and the alloy that described material is comprised of following atomic ratio: (RR ') 1-x(LR 0.9tb 0.1) x(Fe 1-ym y) z, (RR ') represent as Tb 0.27dy 0.73, Tb 0.14ho 0.86traditional magnetocrystalline anisotropy bucking-out system, LR represents light rare earth Pr or Nd, M represents as a kind of or composition of the VIIB of Ni, Co, Mn, VIIIB family element, 0≤x≤0.35 wherein, 0≤y≤0.2,1.85≤z≤2.1.
The present invention also adopts following technical scheme: a kind of preparation technology of giant magnetostriction material of light rare earth modulation, it comprises the steps:
1). raw material preparation: adopt one or several in transition-metal Fe that one or several and purity in rare earth Tb, Dy that purity is 99.9%, Ho, Pr, Nd are 99.9%, Co, Ni, Mn according to stoichiometric equation (RR ') 1-x(LR 0.9tb 0.1) x(Fe 1-ym y) zatomic ratio proportioning;
2). conventional vacuum arc melting: the metal simple-substance that step 1) is obtained is put into the copper crucible in vacuum arc melting furnace chamber, adopt rare earth under, transition metal is at upper modes of emplacement; Close furnace chamber, with mechanical pump, take out in advance and add the continuous mode of taking out of molecular pump, until vacuum degree arrives 10 in furnace chamber -5below Pa, be filled with argon shield gas extremely lower than atmospheric pressure 0.06-0.09MPa; Adopt conventional melting 4 times repeatedly, until alloying component is even;
3). rapid cooling melting: recirculated water is changed to frozen water pattern, and adopting temperature is that the frozen water of 0 degree Celsius is as recirculated water; Electric arc melting alloy is to molten condition, and high speed electromagnetic stirs the alloy material of melting, maintains 10-20 second, closes rapidly arc current, and maintains high speed electromagnetic stirring 5-10 second, treats that material cooled is to room temperature;
4). vacuum annealing: material is taken out and carries out the vacuum annealing 1-15 days time at 300-1000 degree Celsius, obtain well-crystallized's the brilliant giant magnetostriction material of columnar orientation after annealing.
Further, the giant magnetostriction material of described light rare earth modulation has a large amount of column crystals to form along cooling direction.
The present invention has following beneficial effect:
(1) introduce light rare earth and modulate existing heavy rare earth anisotropy bucking-out system, prepared the lower multielement rare earth giant magnetostriction material of magnetocrystalline anisotropy, and adopted cold melting technique one step to obtain partially oriented alloy, and traditional vertical area fusion method of preparing monocrystalline or oriented crystal often needs a large amount of power consumptions and time;
(2) the present invention is simple easily implements, and saves time and energy consumption cost, for efficiently preparing rare earth orientation magnetostrictive material, provides a kind of new approach.
Accompanying drawing explanation:
Fig. 1 is rare earth component (Tb, Dy, Nd) or (Tb, Dy, Pr) phasor (shade represents composition) of polynary giant magnetostriction material.
Fig. 2 is Tb 0.253dy 0.657nd 0.09(Fe 0.9co 0.1) 1.93the section microstructure of column crystal.
Fig. 3 is Tb 0.253dy 0.657nd 0.09(Fe 0.9co 0.1) 1.93column crystal bulk and x-ray diffractogram of powder spectrum.
Fig. 4 is Tb 0.219dy 0.511pr 0.27(Fe 0.9co 0.1) 1.93column crystal bulk and x-ray diffractogram of powder spectrum.
Fig. 5 is the (Tb without orientation 0.27dy 0.73) 1-x(Nd 0.9tb 0.1) x(Fe 0.9co 0.1) 1.93the magnetostriction of alloy and crystal anisotropy constant K 1the ratio of absolute value with composition change curve.
Fig. 6 is Tb 0.253dy 0.657nd 0.09(Fe 0.9co 0.1) 1.93column crystal and without the magnetostriction contrast of orientation alloy.
Embodiment:
Please refer to shown in Fig. 1 to Fig. 6, the present invention is substituted traditional rare earth bucking-out system and is directly obtained the brilliant giant magnetostriction material of columnar orientation by controlling fusion process by light rare earth base bucking-out system trace.
Concrete enforcement is by two class light rare earth base bucking-out system Pr 0.9tb 0.1fe 1.9and Nd 0.9tb 0.1fe 1.9indium addition, make Tb 0.27dy 0.73the magnetocrystalline anisotropy of anisotropy bucking-out system reduces and added cold program one step to obtain oriented material, and wherein transition metal partly adopts 10% the alternative Fe of Co to be optimized.
In order to obtain the brilliant giant magnetostriction material of above-mentioned columnar orientation, the present invention adopts following process, and it comprises the steps:
1). raw material preparation: the transition-metal Fe that rare earth Tb, Dy, Pr, Nd and the purity that employing purity is 99.9% is 99.9% and Co are according to (Tb 0.27dy 0.73) 1-x(Nd 0.9tb 0.1) x(Fe 0.9co 0.1) 1.93(Tb 0.27dy 0.73) 1-x(Pr 0.9tb 0.1) x(Fe 0.9co 0.1) 1.93(atomic ratio) proportioning.Fig. 1 is rare earth component (Tb, Dy, the Nd) phasor (shade represents composition) of polynary giant magnetostriction material;
2). conventional vacuum arc melting: the metal simple-substance that step 1) is obtained is put into the copper crucible in vacuum arc melting furnace chamber, adopt rare earth under, transition metal is at upper modes of emplacement; Close furnace chamber, with mechanical pump, take out in advance and add the continuous mode of taking out of molecular pump, until vacuum degree arrives 10 in furnace chamber -5below Pa, be filled with argon shield gas extremely lower than the about 0.06-0.09MPa of atmospheric pressure; Adopt conventional melting 4 times repeatedly, until alloying component is even;
3). rapid cooling melting: recirculated water is changed to frozen water pattern, and adopting temperature is that the frozen water of 0 degree Celsius is as recirculated water; Electric arc melting alloy is to molten condition, and high speed electromagnetic stirs the alloy material of melting, maintains 10-20 second, closes rapidly arc current, and maintains high speed electromagnetic stirring 5-10 second, treats that material cooled is to room temperature;
4). vacuum annealing: material is taken out and carries out the vacuum annealing 1-15 days time at 300-1000 degree Celsius, and concrete annealing temperature and Time Dependent, in the composition of alloy, obtain well-crystallized's the brilliant giant magnetostriction material of columnar orientation after annealing.
Wherein step 3) recirculated water employing temperature is the frozen water of 0 degree Celsius.The alloy 10-20 of electromagnetic agitation melting will close rapidly arc current after second, and maintains high speed electromagnetic stirring 5-10 second.
The texture of synthetic material with form mutually: by the profile of material, can see along cooling direction and have a large amount of column crystals to form.By the XRD(X x ray diffraction of column crystal bulk and powder) we can see that the diffraction maximum of <110> or <111> direction has had significant enhancing, this showed under cool condition that material was along <110> or <111> direction orientation.
In order better to set forth the process of the brilliant giant magnetostriction material of above-mentioned columnar orientation, below by two specific embodiments, be described in detail.
Embodiment 1
The Tb that is 99.9% by purity, Dy, Nd, 99.9% Fe, Co simple substance are (Tb according to stoichiometric equation 0.27dy 0.73) 1-x(Nd 0.9tb 0.1) x(Fe 0.9co 0.1) 1.93(atomic ratio) proportioning, x span is 0≤x≤0.20.Fig. 1 is rare earth component (Tb, Dy, the Nd) phasor (shade represents composition) of polynary giant magnetostriction material.The raw material preparing is packed in the copper crucible of electric arc melting, copper crucible is adopted and is first used conventional water circulation cooling, adopts electric arc melting to add the mode melt back 4 times of electromagnetic agitation, obtains the uniform alloy mother metal of composition.Recirculated water is changed to frozen water pattern, and adopting temperature is that the frozen water of 0 degree Celsius is as recirculated water; Electric arc melting alloy is to molten condition, and high speed electromagnetic stirs the alloy material of melting, maintains for 10 seconds, closes rapidly arc current, and maintains high speed electromagnetic and stirred for 5 seconds, makes alloy cooling rapidly.Until alloy is down to room temperature, packs material into vacuum annealing furnace and carry out vacuum annealing 5 days.Fig. 2 is that x=0.1 is that materials chemistry formula is Tb 0.253dy 0.657nd 0.09(Fe 0.9co 0.1) 1.93the section micro-structure diagram of material.We can see along cooling direction has a large amount of column crystals to form.X ray diffracting spectrum shows, the direction of these column crystals should be <110> orientation.Fig. 5 is that conventional melting mode obtains the (Tb without orientation that x span is 0≤x≤0.20 0.27dy 0.73) 1-x(Nd 0.9tb 0.1) x(Fe 0.9co 0.1) 1.93magnetostriction and crystal anisotropy constant K 1the ratio of absolute value.We can see that x=0.1 is that materials chemistry formula is Tb 0.253dy 0.657nd 0.090(Fe 0.9co 0.1) 1.93material show optimum magnetostriction character.By contrast, we can see, column crystal material not only effectively raises Magnetostriction in low field, after the match outer at 1.5T, and stroke has reached about 1450ppm.
Embodiment 2
The Tb that is 99.9% by purity, Dy, Nd, 99% Fe, Co simple substance are (Tb according to stoichiometric equation 0.27dy 0.73) 1-x(Pr 0.9tb 0.1) x(Fe 0.9co 0.1) 1.93(atomic ratio) proportioning, x span is 0≤x≤0.35.Fig. 1 is rare earth component (Tb, Dy, the Pr) phasor (shade represents composition) of polynary giant magnetostriction material.The raw material preparing is packed in the copper crucible of electric arc melting, copper crucible is adopted and is first used conventional water circulation cooling, adopts electric arc melting to add the mode melt back 4 times of electromagnetic agitation, obtains the uniform alloy mother metal of composition.Recirculated water is changed to frozen water pattern, and adopting temperature is that the frozen water of 0 degree Celsius is as recirculated water; High speed electromagnetic stirs the alloy material of melting, maintains for 15 seconds, closes rapidly arc current, and maintains high speed electromagnetic and stirred for 10 seconds, until alloy is down to room temperature, packs material into vacuum annealing furnace and carries out vacuum annealing 5 days.Fig. 3 is that x=0.3 is that materials chemistry formula is Tb 0.219dy 0.511pr 0.27(Fe 0.9co 0.1) 1.93the X ray diffracting spectrum of material.XRD shows that the <110> of these column crystal materials and <111> diffraction maximum strengthen to some extent.
The present invention adopts light rare earth base bucking-out system trace to substitute traditional rare earth bucking-out system, simultaneously by transition-metal Fe position is substituted and is optimized, prepared the lower multielement rare earth giant magnetostriction material of anisotropy, and adopted cold melting technique one step to obtain partially oriented alloy, and the preparation process of traditional vertical area fusion method of preparing monocrystalline or oriented crystal often needs a large amount of power consumptions and time.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, can also make some improvement under the premise without departing from the principles of the invention, and these improvement also should be considered as protection scope of the present invention.

Claims (3)

1. the giant magnetostriction material that light rare earth is modulated, is characterized in that: the alloy that described material is comprised of following atomic ratio: (RR ') 1-x(LR 0.9tb 0.1) x(Fe 1-ym y) z, (RR ') represent as Tb 0.27dy 0.73, Tb 0.14ho 0.86traditional magnetocrystalline anisotropy bucking-out system, LR represents light rare earth Pr or Nd, M represents as a kind of or composition of the VIIB of Ni, Co, Mn, VIIIB family element, 0≤x≤0.35 wherein, 0≤y≤0.2,1.85≤z≤2.1.
2. a preparation technology for the giant magnetostriction material that light rare earth is modulated as claimed in claim 1, it comprises the steps:
1). raw material preparation: adopt one or several in transition-metal Fe that one or several and purity in rare earth Tb, Dy that purity is 99.9%, Ho, Pr, Nd are 99.9%, Co, Ni, Mn according to stoichiometric equation (RR ') 1-x(LR 0.9tb 0.1) x(Fe 1-ym y) zatomic ratio proportioning;
2). conventional vacuum arc melting: the metal simple-substance that step 1) is obtained is put into the copper crucible in vacuum arc melting furnace chamber, adopt rare earth under, transition metal is at upper modes of emplacement; Close furnace chamber, with mechanical pump, take out in advance and add the continuous mode of taking out of molecular pump, until vacuum degree arrives 10 in furnace chamber -5below Pa, be filled with argon shield gas extremely lower than atmospheric pressure 0.06-0.09MPa; Adopt conventional melting repeated multiple times, until alloying component is even;
3). rapid cooling melting: recirculated water is changed to frozen water pattern, and adopting temperature is that the frozen water of 0 degree Celsius is as recirculated water; Electric arc melting alloy is to molten condition, and high speed electromagnetic stirs the alloy material of melting, maintains 10-20 second, closes rapidly arc current, and maintains high speed electromagnetic stirring 5-10 second, treats that material cooled is to room temperature;
4). vacuum annealing: material is taken out and carries out the vacuum annealing 1-15 days time at 300-1000 degree Celsius, obtain well-crystallized's the brilliant giant magnetostriction material of columnar orientation after annealing.
3. the preparation technology of the giant magnetostriction material of light rare earth modulation as claimed in claim 2, is characterized in that: described giant magnetostriction material has a large amount of column crystals to form along cooling direction.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110423932A (en) * 2019-08-23 2019-11-08 南京信息职业技术学院 A kind of magnetostriction materials and preparation method of light rare earth Pr doping
CN111057959A (en) * 2019-12-05 2020-04-24 南京信息职业技术学院 Magnetostrictive material and preparation process thereof
CN111378906A (en) * 2020-04-14 2020-07-07 聊城大学 Ultrahigh hypersensitive magnetostrictive material
WO2020228709A1 (en) * 2019-05-15 2020-11-19 刘丽 Method for preparing alloy powder material
CN112575237A (en) * 2020-12-09 2021-03-30 南京航空航天大学 Co-Ni-Mn-Si-Tb giant magnetostrictive material and preparation method thereof

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CN1705761A (en) * 2002-10-25 2005-12-07 昭和电工株式会社 Alloy containing rare earth element, production method thereof, magnetostrictive device, and magnetic refrigerant material

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CN1705761A (en) * 2002-10-25 2005-12-07 昭和电工株式会社 Alloy containing rare earth element, production method thereof, magnetostrictive device, and magnetic refrigerant material
CN1648265A (en) * 2004-01-26 2005-08-03 Tdk株式会社 Method for producing magnetostrictive material

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唐少龙，吴昌衡，金希梅，王博文，庄育智，李强，李靖元: "Dy0.6Tb0.3Pr0.1(Fe0.95Mn0.05)x取向晶体的结构与磁致伸缩", 《功能材料》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020228709A1 (en) * 2019-05-15 2020-11-19 刘丽 Method for preparing alloy powder material
CN110423932A (en) * 2019-08-23 2019-11-08 南京信息职业技术学院 A kind of magnetostriction materials and preparation method of light rare earth Pr doping
CN111057959A (en) * 2019-12-05 2020-04-24 南京信息职业技术学院 Magnetostrictive material and preparation process thereof
CN111378906A (en) * 2020-04-14 2020-07-07 聊城大学 Ultrahigh hypersensitive magnetostrictive material
CN112575237A (en) * 2020-12-09 2021-03-30 南京航空航天大学 Co-Ni-Mn-Si-Tb giant magnetostrictive material and preparation method thereof

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