CN103647019B - The giant magnetostriction material of a kind of light rare earth modulation and preparation technology thereof - Google Patents
The giant magnetostriction material of a kind of light rare earth modulation and preparation technology thereof Download PDFInfo
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- CN103647019B CN103647019B CN201310617774.4A CN201310617774A CN103647019B CN 103647019 B CN103647019 B CN 103647019B CN 201310617774 A CN201310617774 A CN 201310617774A CN 103647019 B CN103647019 B CN 103647019B
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- 239000000463 material Substances 0.000 title claims abstract description 67
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 49
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims description 17
- 238000005516 engineering process Methods 0.000 title claims description 9
- 238000002844 melting Methods 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 14
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 11
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 7
- 239000000956 alloy Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910045601 alloy Inorganic materials 0.000 claims description 23
- 238000000137 annealing Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 229910052771 Terbium Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010891 electric arc Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 150000003624 transition metals Chemical class 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052723 transition metal Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 238000007499 fusion processing Methods 0.000 abstract description 4
- 238000013459 approach Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000002269 spontaneous effect Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000007500 overflow downdraw method Methods 0.000 description 3
- -1 AlN compound Chemical class 0.000 description 1
- 229910001329 Terfenol-D Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000005486 microgravity Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The present invention provides a kind of trace to add light rare earth to conventional compensation system and by controlling the method that fusion process directly obtains columnar orientation crystalline substance giant magnetostriction material.The method utilizes big Spontaneous magnetostriction and the feature of low magnetocrystalline anisotropy of light rare earth Pr and Nd, existing compensation system is optimized, and in melting, add supercool program, directly obtain and there is the Rare-Earth Giant Magnetostrictive Materials that part<100>or<111>is orientated.The method is simple, time-consuming and energy consumption cost, provides a kind of approach for quickly preparing oriented crystal.
Description
Technical field:
The present invention relates to giant magnetostriction material and the preparation technology thereof of 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, is primarily referred to as RFe2(R=rare earth) rare earth
Cubic AlN compound between metal.The efficient conversion that this kind of material is capable of between electromagnetic energy and mechanical energy.The U.S.
The O.D.McMasters of the A.E.Clark in naval surface weapon research center etc. and USDOE's Ames Lab
Cooperation, is compensated by magnetocrystalline anisotropy between rare earth, has obtained not only having big low field magnetostriction but also have low
The Tb of magnetocrystalline anisotropy0.27Dy0.73Fe2Alloy.This invention be applied as Patent No. US3949351 and
The United States Patent (USP) of US4308474.At the end of the eighties, the RTREMA company of famous American with this counterfeit dualization alloy is
Basis makes rare earth giant magnetostrictive material commercialization, its product designation Terfenol-D.Traditional rare earth giant magnetostrictive driver material
The preparation technology of material is grasped by the U.S., mostly such as Patent No. US4609402 of 1986, the Patent No. of 1988
US4770704, the United States Patent (USP) of Patent No. US4818304 of 1989 disclose respectively vertical area fusion method,
The method that pulling method, magnetic-field annealing method etc. prepare rare earth giant magnetostrictive material.Within 2002, Japanese researchers utilizes microgravity bar
<111>orientation TbDyFe alloy is obtained under part.China Patent Publication No. CN1232275A rare-earth-iron super magnetostriction material
Material and manufacturing process provide a kind of prepare<110>and are oriented to main manufacturing process.China Patent Publication No.
CN1435851A giant magnetostriction material and manufacturing process provide one<113>and are oriented to main giant magnetostriction material
Manufacturing process.Although the magnetoelastic properties of the material that directional solidification method obtains is significantly improved, but preparation orientation
Alloy, need first to obtain alloy mother metal and then regrow at crystal growing furnace and pilot process length, can not be interrupted, make
The preparation cost obtaining material increases and the longest.
Single ion model calculates and shows PrFe2Spontaneous magnetostriction coefficient lambda at absolute zero111Reach 5600ppm, than
TbFe2(λ111=4400ppm) and DyFe2(λ111=4200ppm) there is higher theoretical magnetostriction value.And NdFe2
The magnetostriction coefficient of absolute zero is also reached 2000ppm, compares HoFe2(λ111=1600ppm) big 25%.
Additionally, the resource of light rare earth Pr, Nd is abundanter, than the low price of heavy rare earth.So many work are devoted to light
The exploitation of rare earth giant magnetostrictive material, CN1096546 as open in Chinese patent, CN1125265, CN1232275,
CN1435851 etc. all take partially substituted method to be added to by Pr in the counterfeit dualization alloy of TbDyFe base, it is intended that
Obtain the new material of high Pr content high-magnetostriction.But the light rare earth of excess adds membership and causes the generation of the second phase, sternly
Ghost image rings the magnetoelastic properties of material.We find in the development process of light rare earth giant magnetostriction material, appropriate
Light rare earth Pr, Nd introduce the magnetocrystalline anisotropy that can effectively reduce TbDyFe base magnetic striction material.Additionally, I
Can directly obtain partially oriented magnetostriction materials by controlling fusion process, so make keeping material excellent
While Magnetostriction, the preparation cost of material is greatly reduced.
Summary of the invention:
The present invention provides the giant magnetostriction material and preparation technology thereof that a kind of light rare earth modulates.Light rare earth base is used to compensate system
System trace substitutes traditional rare earth and compensates system and control fusion process and directly obtain columnar orientation crystalline substance giant magnetostriction material.
The present invention adopts the following technical scheme that the giant magnetostriction material that a kind of light rare earth is modulated, and described material is by the most former
Son is than the alloy of composition: (RR ')1-x(LR0.9Tb0.1)x(Fe1-yMy)z, (RR ') represent such as Tb0.27Dy0.73、Tb0.14Ho0.86's
Tradition magnetocrystalline anisotropy compensates system, LR represent light rare earth Pr or Nd, M represent such as Ni, Co, Mn VIIB,
The one of group VIIIB element or composition, wherein 0≤x≤0.35,0≤y≤0.2,1.85≤z≤2.1.
The present invention also adopts the following technical scheme that the preparation technology of the giant magnetostriction material that a kind of light rare earth modulates, its bag
Include following steps:
1). preparation of raw material: employing purity is one or several in rare earth Tb, Dy, Ho, Pr, Nd of 99.9%
With one or several in the transition-metal Fe that purity is 99.9%, Co, Ni, Mn according to stoichiometric equation
(RR’)1-x(LR0.9Tb0.1)x(Fe1-yMy)zAtomic ratio proportioning;
2). conventional vacuum arc melting: by step 1) metal simple-substance that obtains puts into the copper of vacuum arc melting furnace intracavity
In crucible, use rare earth under, transition metal is at upper modes of emplacement;Close furnace chamber, take out in advance with mechanical pump and add molecular pump
The continuous mode taken out, until vacuum arrives 10 in furnace chamber-5Below Pa, is filled with argon shield gas to subatmospheric
0.06-0.09MPa;Use conventional melting 4 times repeatedly, until alloying component is uniform;
3). rapid cooling melting: recirculated water shifts to frozen water pattern, i.e. using temperature is that the frozen water of 0 degree Celsius is as recirculated water;
Electric arc melting alloy, to molten condition, the alloy material that high speed electromagnetic stirring is melted, maintains 10-20 second, closes rapidly
Arc current, and maintain high speed electromagnetic to stir 5-10 second, treat that material is cooled to room temperature;
4). vacuum annealing: material is taken out and carries out the 1-15 days time of vacuum annealing at 300-1000 degree Celsius, annealing
After obtain the columnar orientation crystalline substance giant magnetostriction material of well-crystallized.
Further, the giant magnetostriction material of described light rare earth modulation has substantial amounts of column crystal to be formed along cooling direction.
There is advantages that
(1) introduce light rare earth and modulate existing heavy rare earth anisotropy compensation system, be prepared for magnetocrystalline anisotropy lower
Multielement rare earth giant magnetostriction material, and use supercool melting technique one step to obtain partially oriented alloy, and traditional
The vertical area fusion method preparing monocrystalline or oriented crystal generally requires substantial amounts of power consumption and time;
(2) present invention the most easily implements, time-consuming and energy consumption cost, for efficiently preparing rare earth orientation magnetostriction
Material provides a kind of new approach.
Accompanying drawing illustrates:
Fig. 1 is rare earth component (Tb, Dy, Nd) or (Tb, Dy, Pr) phasor (face of polynary giant magnetostriction material
Color depth is shallow represents composition).
Fig. 2 is Tb0.253Dy0.657Nd0.09(Fe0.9Co0.1)1.93The section microstructure of column crystal.
Fig. 3 is Tb0.253Dy0.657Nd0.09(Fe0.9Co0.1)1.93Column crystal bulk and x-ray diffractogram of powder spectrum.
Fig. 4 is Tb0.219Dy0.511Pr0.27(Fe0.9Co0.1)1.93Column crystal bulk and x-ray diffractogram of powder spectrum.
Fig. 5 is the (Tb of No yield point0.27Dy0.73)1-x(Nd0.9Tb0.1)x(Fe0.9Co0.1)1.93The magnetostriction of alloy and magnetocrystalline
Opposite sex constant K1The ratio of absolute value with composition transfer curve.
Fig. 6 is Tb0.253Dy0.657Nd0.09(Fe0.9Co0.1)1.93The magnetostriction contrast of column crystal and No yield point alloy.
Detailed description of the invention:
Refer to shown in Fig. 1 to Fig. 6, the present invention compensates system trace by light rare earth base and substitutes traditional rare earth compensation system
And directly obtain columnar orientation crystalline substance giant magnetostriction material by controlling fusion process.
It is embodied as being to compensate system Pr by two class light rare earth bases0.9Tb0.1Fe1.9And Nd0.9Tb0.1Fe1.9Trace add,
Make Tb0.27Dy0.73Anisotropy compensates the magnetocrystalline anisotropy of system and reduces and add supercool program one step and taken
To material, wherein transition metal moieties uses the Co replacement Fe of 10% to be optimized.
In order to obtain above-mentioned columnar orientation crystalline substance giant magnetostriction material, the present invention uses following process, and it includes as follows
Step:
1). preparation of raw material: rare earth Tb, Dy, Pr, the Nd and the purity that use purity to be 99.9% are the transition of 99.9%
Metal Fe and Co is according to (Tb0.27Dy0.73)1-x(Nd0.9Tb0.1)x(Fe0.9Co0.1)1.93With
(Tb0.27Dy0.73)1-x(Pr0.9Tb0.1)x(Fe0.9Co0.1)1.93(atomic ratio) proportioning.Fig. 1 is polynary giant magnetostriction material
Rare earth component (Tb, Dy, Nd) phasor (shade represents composition);
2). conventional vacuum arc melting: by step 1) metal simple-substance that obtains puts into the copper of vacuum arc melting furnace intracavity
In crucible, use rare earth under, transition metal is at upper modes of emplacement;Close furnace chamber, take out in advance with mechanical pump and add molecular pump
The continuous mode taken out, until vacuum arrives 10 in furnace chamber-5Below Pa, is filled with argon shield gas to subatmospheric about
0.06-0.09MPa;Use conventional melting 4 times repeatedly, until alloying component is uniform;
3). rapid cooling melting: recirculated water shifts to frozen water pattern, i.e. using temperature is that the frozen water of 0 degree Celsius is as recirculated water;
Electric arc melting alloy, to molten condition, the alloy material that high speed electromagnetic stirring is melted, maintains 10-20 second, closes rapidly
Arc current, and maintain high speed electromagnetic to stir 5-10 second, treat that material is cooled to room temperature;
4). vacuum annealing: material is taken out and carries out the 1-15 days time of vacuum annealing, specifically at 300-1000 degree Celsius
Annealing temperature and time-dependent, in the composition of alloy, obtain the columnar orientation crystalline substance giant magnetostriction material of well-crystallized after annealing.
Wherein step 3) recirculated water uses temperature to be the frozen water of 0 degree Celsius.After the alloy 10-20 second that electromagnetic agitation is melted
To close rapidly arc current, and maintain high speed electromagnetic to stir 5-10 second.
The texture of synthetic material is with composition mutually: by the profile of material, it can be seen that have substantial amounts of post along cooling direction
Shape crystalline substance is formed.By the XRD (X-ray diffraction) of column crystal bulk and powder it may be seen that<110>or<111>
The diffraction maximum in direction has had significant enhancing, this show supercool under the conditions of material along<110>or<111>direction be orientated.
In order to preferably illustrate the process of above-mentioned columnar orientation crystalline substance giant magnetostriction material, concrete below by two
Embodiment is described in detail.
Embodiment 1
Being Tb, Dy, Nd of 99.9% by purity, Fe, Co simple substance of 99.9% according to stoichiometric equation is
(Tb0.27Dy0.73)1-x(Nd0.9Tb0.1)x(Fe0.9Co0.1)1.93(atomic ratio) proportioning, x span is 0≤x≤0.20.Fig. 1
Rare earth component (Tb, Dy, Nd) phasor (shade represents composition) for polynary giant magnetostriction material.Will preparation
Good raw material loads in the copper crucible of electric arc melting, and copper crucible, initially with conventional water circulating cooling, uses electric arc melting to add
The mode melt back of electromagnetic agitation 4 times, obtains composition uniform alloy mother metal.Recirculated water is shifted to frozen water pattern, i.e.
Using 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 stirring is melted
Alloy material, maintain 10 seconds, close rapidly arc current, and maintain high speed electromagnetic to stir 5 seconds, allow alloy
Cooling rapidly.Until room temperature is down to by alloy, loads material into vacuum annealing furnace and carry out vacuum annealing 5 days.Fig. 2 is x=0.1
I.e. materials chemistry formula is Tb0.253Dy0.657Nd0.09(Fe0.9Co0.1)1.93The section micro-structure diagram of material.It may be seen that
Substantial amounts of column crystal is had to be formed along cooling direction.Fig. 3 is Tb0.253Dy0.657Nd0.09(Fe0.9Co0.1)1.93Column crystal bulk
Compose with x-ray diffractogram of powder.X ray diffracting spectrum shows, the direction of these column crystals should be<110>orientation.
Fig. 5 is that conventional melting mode obtains the No yield point that x span is 0≤x≤0.20
(Tb0.27Dy0.73)1-x(Nd0.9Tb0.1)x(Fe0.9Co0.1)1.93Magnetostriction and crystal anisotropy constant K1Absolute value
Ratio.It may be seen that x=0.1 i.e. materials chemistry formula is Tb0.253Dy0.657Nd0.090(Fe0.9Co0.1)1.93Material represent
Go out the magnetoelastic properties of optimum.Fig. 6 is Tb0.253Dy0.657Nd0.09(Fe0.9Co0.1)1.93Column crystal and No yield point alloy
Magnetostriction contrasts.By contrast, stretch it will be seen that column crystal material not only effectively raises mangneto in low field
Contracting performance, 1.5T outer after the match, stroke has reached about 1450ppm.
Embodiment 2
Being Tb, Dy, Pr of 99.9% by purity, Fe, Co simple substance of 99% according to stoichiometric equation is
(Tb0.27Dy0.73)1-x(Pr0.9Tb0.1)x(Fe0.9Co0.1)1.93(atomic ratio) proportioning, x span is 0≤x≤0.35.Fig. 1
Rare earth component (Tb, Dy, Pr) phasor (shade represents composition) for polynary giant magnetostriction material.Will preparation
Good raw material loads in the copper crucible of electric arc melting, and copper crucible is adopted first by conventional water circulating cooling, uses electric arc melting to add
The mode melt back of electromagnetic agitation 4 times, obtains composition uniform alloy mother metal.Recirculated water is shifted to frozen water pattern, i.e.
Using temperature is that the frozen water of 0 degree Celsius is as recirculated water;The alloy material that high speed electromagnetic stirring is melted, maintains 15 seconds,
Close rapidly arc current, and maintain high speed electromagnetic to stir 10 seconds, until room temperature is down to by alloy, load material into true
Empty annealing furnace carries out vacuum annealing 5 days.Fig. 4 is that x=0.3 i.e. materials chemistry formula is
Tb0.219Dy0.511Pr0.27(Fe0.9Co0.1)1.93The X ray diffracting spectrum of material.XRD shows these column crystal materials
<110>strengthened with<111>diffraction maximum.
The present invention uses light rare earth base to compensate system trace and substitutes traditional rare earth compensation system, simultaneously by transition metal
Fe position substitutes and optimizes, and is prepared for the multielement rare earth giant magnetostriction material that anisotropy is relatively low, and uses supercool melting technique
One step obtains partially oriented alloy, and the preparation of traditional vertical area fusion method preparing monocrystalline or oriented crystal
Journey generally requires substantial amounts of power consumption and time.
The above is only the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, some improvement can also be made under the premise without departing from the principles of the invention, these improvement also should be regarded as the present invention's
Protection domain.
Claims (2)
1. the preparation technology of the giant magnetostriction material of a light rare earth modulation, it is characterised in that comprise the steps:
1). preparation of raw material: employing purity is one or several in rare earth Tb, Dy, Ho, Pr, Nd of 99.9%
With one or several in the transition-metal Fe that purity is 99.9%, Co, Ni, Mn according to stoichiometric equation
(RR’)1-x(LR0.9Tb0.1)x(Fe1-yMy)zAtomic ratio proportioning, and wherein (RR ') it is Tb0.27Dy0.73、Tb0.14Ho0.86Tradition
Magnetocrystalline anisotropy compensates system, and LR is light rare earth Pr or Nd, and M is VIIB, VIIIB of Ni, Co, Mn
The one of race's element or composition, wherein 0≤x≤0.35,0≤y≤0.2,1.85≤z≤2.1;
2). conventional vacuum arc melting: by step 1) metal simple-substance that obtains puts into the copper of vacuum arc melting furnace intracavity
In crucible, use rare earth under, transition metal is at upper modes of emplacement;Close furnace chamber, take out in advance with mechanical pump and add molecular pump
The continuous mode taken out, until vacuum arrives 10 in furnace chamber-5Below Pa, is filled with argon shield gas to subatmospheric
0.06-0.09MPa;Use conventional melting repeated multiple times, until alloying component is uniform;
3). rapid cooling melting: recirculated water shifts to frozen water pattern, i.e. using temperature is that the frozen water of 0 degree Celsius is as recirculated water;
Electric arc melting alloy, to molten condition, the alloy material that high speed electromagnetic stirring is melted, maintains 10-20 second, closes rapidly
Arc current, and maintain high speed electromagnetic to stir 5-10 second, treat that material is cooled to room temperature;
4). vacuum annealing: material is taken out and carries out the 1-15 days time of vacuum annealing at 300-1000 degree Celsius, annealing
After obtain the columnar orientation crystalline substance giant magnetostriction material of well-crystallized.
2. the preparation technology of the giant magnetostriction material of light rare earth modulation as claimed in claim 1, it is characterised in that: institute
Stating giant magnetostriction material has substantial amounts of column crystal to be formed along cooling direction.
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CN111057959A (en) * | 2019-12-05 | 2020-04-24 | 南京信息职业技术学院 | Magnetostrictive material and preparation process thereof |
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CN112575237B (en) * | 2020-12-09 | 2021-11-02 | 南京航空航天大学 | Co-Ni-Mn-Si-Tb giant magnetostrictive material and preparation method thereof |
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US6508854B2 (en) * | 2000-09-12 | 2003-01-21 | National Institute Of Advanced Industrial Science And Technology | Method of preparing magnetostrictive material in microgravity environment |
CN1648265A (en) * | 2004-01-26 | 2005-08-03 | Tdk株式会社 | Method for producing magnetostrictive material |
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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US6508854B2 (en) * | 2000-09-12 | 2003-01-21 | National Institute Of Advanced Industrial Science And Technology | Method of preparing magnetostrictive material in microgravity environment |
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 |
Non-Patent Citations (1)
Title |
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Dy0.6Tb0.3Pr0.1(Fe0.95Mn0.05)x取向晶体的结构与磁致伸缩;唐少龙,吴昌衡,金希梅,王博文,庄育智,***,李靖元;《功能材料》;20040108;第31卷(第3期);第259页至第261页 * |
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