CN101826385A - Magnetic material with exchange bias effect and preparation method thereof - Google Patents

Magnetic material with exchange bias effect and preparation method thereof Download PDF

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CN101826385A
CN101826385A CN 201010164927 CN201010164927A CN101826385A CN 101826385 A CN101826385 A CN 101826385A CN 201010164927 CN201010164927 CN 201010164927 CN 201010164927 A CN201010164927 A CN 201010164927A CN 101826385 A CN101826385 A CN 101826385A
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magnetic
magnetic material
exchange bias
bias effect
temperature
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马丽
陈京兰
王文洪
吴光恒
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Institute of Physics of CAS
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Abstract

The invention discloses a magnetic material with exchange bias effect and a preparation method thereof. The chemical formula of the magnetic material is MnmNinSno, wherein m is more than or equal to 30 and less than 55, n is more than or equal to 25 and less than or equal to 50, o is more than or equal to 9 and less than 13, the sum of the m, the n and the o is 100, and the m, the n and the o express atomic percent contents. The preparation method for the magnetic material comprises the following steps: (1) weighing raw materials according to the chemical formula MnmNinSno; and (2) putting the weighed raw materials into a crucible, and preparing MnmNinSno magnetic monocrystal or polycrystal by adopting a conventional pulling method or an electric arc smelting method and a quick quenching strip-throwing method. Compared with the existing alloy, the magnetic material MnmNinSno has larger exchange bias field HE value and higher magnetic field controllability, and can be used for manufacturing drivers, temperature and/or magnetic sensitive elements, magnetic refrigerating devices and equipment, magnetic memories, micro electromechanical devices and systems and the like.

Description

A kind of magnetic material and preparation method thereof with exchange bias effect
Technical field
The present invention relates to a kind of shape-memory material, have ferromagnetism and bidirectional shape memory effect, particularly relate to MnNiSn magnetic material with big exchange bias effect and preparation method thereof.
Background technology
The general shape memorial alloy has a kind of crystal structure (hereinafter referred to as parent phase) under high relatively temperature, and under low relatively temperature spontaneous another crystal structure that becomes, generally be referred to as martensitic phase.When from higher greenhouse cooling to lower temperature, material changes martensitic phase into from parent phase, and this changes mutually and is called martensitic phase transformation.Conversely, from low relatively temperature heating material, alloy can change parent phase into from martensitic phase, and this opposite transformation mutually is called the martensite reverse transformation.Generally, be called M with the starting point and the terminal point of martensite transfor mation sPoint and M fPoint, beginning and terminal point with the martensite reverse transformation are called A sPoint and A fThe point.If M sAnd A sBetween difference less, such as be the several years or tens the degree, this martensitic phase transformation of material is called as thermoelastic martensitic transformation.
Usually, certain alloy material is cooled off with the shape of determining at parent phase, behind martensitic phase, change original shape more artificially, then, alloy material is heated up, when being transformed into austenite, if the shape of alloy material completely or partially changes original shape into, this phenomenon is called shape memory effect.In addition, if in the circulation of same said temperature, the shape of parent phase is out of shape constantly in the phase transformation that cooling causes, the reverse transformation redeformation constantly that causes in subsequently intensification again, and partly or entirely be transformed into the shape of original parent phase, be referred to as bidirectional shape memory effect.
Type purposes that marmem is widely used in various " intelligence ", as various drivers, temperature-sensing element (device), medicine equipment etc.
1956, Meikleijohn and Bean at first observed exchange biased phenomenon first in Co (ferromagnetic material) particle system that CoO (antiferromagnet) shell covers.When system added the N of magnetic field by antiferromagnet CoO and is cooled to 77K, the magnetic hysteresis loop of sample was along the reverse deviation from origin of cooling field direction, and the coercitive increase of simultaneous, at that time this phenomenon is referred to as exchange bias effect.Its physical mechanism is as follows: (between TN＜T＜TC), ferromagnet is in ordered magnetic state in the system, and its magnetic moment forwards the direction that is parallel to the outfield under the action of a magnetic field when system temperature is in the N TN of antiferromagnet and the Curie temperature TC of ferromagnetic material; And antiferromagnet is in paramagnetic state at this moment, and its inner magnetic moment is a disorder distribution.When system is cooled to below the N under magnetic field, at this moment antiferromagnet also enters ordered magnetic state.Because at the ferromagnetic one antiferromagnetic exchange interaction that exists at the interface, antiferromagnet atomic magnetic moment at the interface will the parallel or antiparallel ground arrangement (depending on exchange integral Jex) along ferromagnetic magnetic moment direction.So just in the process that forms interface spin pinning layer at the interface.When externally-applied magnetic field reversed, ferromagnetic magnetic moment is outer field reversal and then, and for antiferromagnet, each is very big to different magnetic constant to it is generally acknowledged it, and spin magnetic moment does not change with the outfield at the interface.Because interface coupling, antiferromagnet attempt to allow ferromagnetic magnetic moment still remain on the direction of original cooling field.Therefore when measurement magnetic field was opposite with the cooling field direction, ferromagnetic magnetic moment was than difficult upset, and coercive force is bigger.When measurement magnetic field was consistent with the cooling field direction, ferromagnetic magnetic moment was easy to turn to parallel with it direction, and coercive force is less; So on macroscopic view, show as the opposite direction skew of magnetic hysteresis loop, present unidirectional anisotropy along the cooling field.
Since finding this phenomenon, in the spintronics field that develops rapidly, the extensive use in permanent magnet, super-high density magnetic recording media, magnetic reading head, giant magnetoresistance, Spin Valve, the novel memory of tunnel junction and transducer of the pinning effect of exchange bias effect.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of magnetic material with big exchange bias effect, and this magnetic material not only has the character of common shape-memory material phase transformation, and has big exchange biased phenomenon in its martensitic phase.The magnetic field controllability of material is improved greatly, and range of application is more extensive.Further aim of the present invention is, a kind of above-mentioned this method with magnetic material of big exchange bias effect for preparing also is provided.
For achieving the above object, the present invention has the magnetic material of exchange bias effect, and its chemical formula is: Mn mNi nSn oWherein, 30≤m＜55,25≤n≤50,9≤o＜13, m+n+o=100, m, n, o represent atom percentage content.
Further, described Mn mNi nSn oThe form of magnetic material comprises mono-crystalline structures and polycrystalline structure.
The preparation method of the magnetic material monocrystalline with exchange bias effect that the present invention proposes comprises the steps:
(1) presses chemical formula Mn mNi nSn oRaw materials weighing, wherein, 30≤m＜55,25≤n≤50,9≤o＜13, m+n+o=100, m, n, o represent atom percentage content;
(2) material that will weigh up is contained in the crucible, adopts conventional Czochralski grown Mn mNi nSn oMagnetic mono crystal, its growth conditions is: the heating mentioned component former expect make it fusion; Its fusion environment is 1 * 10 -2To 5 * 10 -5The argon shield gas of the vacuum of Pa or 0.01～1MPa normal pressure; A seed crystal is fixed in seed rod lower end with 0.5～50 rev/min speed rotation; Described seed crystal is a composition monocrystalline identical or approaching, that have needed orientation;
(3) under 1000～1200 ℃ melt temperature condition, kept 10～30 minutes, liquid level with end in contact melt under the seed crystal, with 3～80mm/ hour uniform rate lifting seed rod, lift on the single crystal direction with solidification and crystallization then, and make the single crystal diameter of growth become big or keep certain;
(4) when the monocrystalline of growth reaches required size, single crystal pulling is broken away from the raw material surface of fusion, slowly reduce temperature with 0.5～20 ℃/minute rate of temperature fall and be cooled to room temperature, take out at last.
Further, the above-mentioned sample for preparing was annealed in 500～1200 ℃ temperature range 0.01～100 hour again, and then cool off with 0.01～1000 ℃/second rate of temperature fall.
Described growth mode of heating can heat or the resistance heating mode with the radio frequency of 50～245 KHz.Described crucible can be magnetic levitation cold crucible, graphite crucible or silica crucible.
The preparation method of the magnetic material polycrystalline with exchange bias effect that the present invention proposes comprises the steps:
(1) presses chemical formula Mn mNi nSn oRaw materials weighing, wherein, 30≤m＜55,25≤n≤50,9≤o＜13, m+n+o=100, m, n, o represent atom percentage content;
(2) material that will weigh up is contained in the melting kettle, adopts the electric arc melting method to obtain Mn mNi nSn oThe magnetic polycrystalline, its melting condition is: reach 2 * 10 in vacuum -3When Pa is following, feed 0.1～1.2MPa argon gas, whole fusion process sample adopts argon shield, melting electric current 30～100A, and congruent melting refining four times is even to guarantee composition; After the smelted product that is obtained wraps up with tantalum piece, pack in the vitreosil pipe that seals, in 500～1200 ℃ temperature range, annealed 0.1～100 hour, and then cool off with 0.01～1000 ℃/second rate of temperature fall, arrange taking-up at last to realize the atom high-sequential.
Further, the alloy that obtains at last in the step (2) is put into the quartz ampoule that gets rid of the band machine, be evacuated down to 10 -3More than the Pa, get rid of the interior high-purity argon gas that feeds of furnace chamber of band machine, pressure is 0.05MPa, adopt induction heating, make alloy be in molten condition, be blown into the high-purity argon gas that pressure is 0.1～1.2MPa then from quartz ampoule top, molten alloy liquid is ejected into from aperture on the copper wheel of high speed rotating that linear velocity is 10～30m/s throws away fast, adopting this fast quenching to get rid of band method acquisition width is 1-10mm, and thickness is the polycrystalline state alloy material of 40-50 μ m.
Magnetic material with big exchange bias effect provided by the invention, it shows the characteristic value exchange bias field H of exchange bias effect ECan be by changing Mn, Ni, Sn ratio of components and change or adjusted according to purposes.This material under martensitic state because the increase of the cooling field that adds can make magnetic hysteresis loop be moved to the negative semiaxis in magnetic field fully.Thereby show strong uniaxial magnetic anisotropy.So, the magnetic material Mn with big exchange bias effect provided by the invention mNi nSn oHas purposes widely, driver for example, temperature and/or magnetic senser, magnetic refrigeration device and equipment, magnetic memory, micro-electro-mechanical device and system etc.
Description of drawings
Fig. 1 is Mn of the present invention mNi nSn oMaterial exchange bias effect figure.
Embodiment
Mn of the present invention mNi nSn oThe exchange bias effect of magnetic material as shown in Figure 1.
Embodiment 1
Preparation consists of: Mn 40Ni 50Sn 10The magnetic alloy with exchange bias effect; adopting growth parameter(s) is the radio frequency heating of 245 KHz, arrives the argon gas of 1MPa normal pressure as protective gas, in magnetic levitation cold crucible with 0.01; heating power is 20 kilowatts, and its preparation method is undertaken by following concrete steps:
(1) weighing purity respectively is 99.9% Mn, Ni, Sn;
(2) material that will weigh up is put into crucible, is heated to 1200 ℃ of fusions, keeps 10～30 minutes;
(3) with the NiMnSn[001 of 2 * 2 * 7mm size] oriented single crystal is the seeded growth monocrystalline; The seed rod speed of rotation is 30 rev/mins in its growth course, and pulling growth speed is 30mm/ hour;
(4) be 10 millimeters when obtaining diameter, when length is 100 millimeters high quality single crystal, single crystal pulling broken away from the raw material surface of fusion, slowly reduce temperature with 0.5～20 ℃/minute rate of temperature fall and be cooled to room temperature, take out at last;
(5) sample for preparing was annealed in 500-1200 ℃ temperature range 0.01～100 hour again, and then cool off with 0.01～1000 ℃/second rate of temperature fall.
Monocrystalline is cut into the small sample of 4 * 4 * 8mm and the large sample of 10 * 10 * 100mm along [001] direction, measure above-mentioned various character, obtain the various characteristics curve, respective value sees Table 1.
Embodiment 2
Preparation consists of: Mn 45Ni 45Sn 10Magnetic alloy with exchange bias effect; Different is in silica crucible, is heated by resistive the method growth, and removing the seed rod speed of rotation is 20 rev/mins, and pulling growth speed is outside 20mm/ hour, and all the other measure above-mentioned various character with embodiment 1, obtain the various characteristics curve, and respective value sees Table 1.
Embodiment 3
Preparation consists of: Mn 47Ni 40Sn 13The magnetic alloy with exchange bias effect; Removing the seed rod speed of rotation is 10 rev/mins, and pulling growth speed is outside 50mm/ hour, and all the other are with embodiment 1.Measure above-mentioned various character, obtain the various characteristics curve, respective value sees Table 1.
Embodiment 4
Preparation consists of: Mn 50Ni 40Sn 10The magnetic alloy with exchange bias effect, adopt the electric arc melting method, as protective gas, in the copper crucible of water-cooled, heating current is 100A with the argon gas of 0.1MPa normal pressure, its preparation method is undertaken by following concrete steps:
(1) weighing purity respectively is 99.9% Mn, Ni, Sn;
(2) material that will weigh up is put into copper crucible, puts into smelting furnace, with mechanical pump forvacuum to 5 * 10 -1Pa;
(3) be evacuated down to 1 * 10 with molecular pump -4Pa feeds high-purity argon gas, makes melting chamber internal pressure reach 0.1MPa;
(4) produce electric arc, the electric arc head remains on 2-5cm place, sample top and swings about 1min repeatedly among a small circle, and the metal of the above-mentioned weighing of melt back four times is so that the alloying component of preparation is even; Treat that furnace chamber is cooled to room temperature, take out at last;
(5) with the alloy for preparing again 800 ℃ annealing temperature 72 hours, and then with 0.01～1000 ℃/second rate of temperature fall cooling.
Utilize line to be cut into the small sample of 4 * 4 * 8mm and the large sample of 10 * 10 * 100mm in above-mentioned polycrystalline sample, measure various character, obtain the various characteristics curve, respective value sees Table 1.
Embodiment 5
Preparation consists of: Mn 55Ni 36Sn 9The magnetic alloy with exchange bias effect, its preparation method is measured various character with embodiment 4, obtains the various characteristics curve, empirical value sees Table 1.
Embodiment 6
Preparation consists of: Mn 30Ni 48Sn 12The magnetic alloy with exchange bias effect, adopt fast quenching to get rid of the band method, as protective gas, its preparation method is undertaken by following concrete steps with the argon gas of 0.05MPa normal pressure:
(1) suitably the alloy that above-mentioned method of smelting prepares that passes through of size is put into the quartz ampoule that a bottom has aperture, is placed to and gets rid of in the band machine furnace chamber;
(2) be evacuated down to 10 -3Below the Pa, feed high-purity argon gas in the furnace chamber, pressure is 0.05MPa;
(3) adopt induction heating, constantly regulate the power of induction heating, make alloy be in white molten condition of processing, be blown into high-purity argon gas, molten alloy liquid is ejected into from aperture on the copper wheel of high speed rotating that linear velocity is 17m/s throws away fast with certain pressure from quartz ampoule top.
Measure above-mentioned various character of getting rid of carry sample, obtain the various characteristics curve, respective value sees Table 1.
The Mn of table 1 heterogeneity mNi nSn oThe H of material under 1000Oe cooling field and 5K low temperature ENumerical value, H CValue
Composition ??H E??(Oe) ??H C??(Oe)
??Mn 40Ni 50Sn 10 ??476 ??167
??Mn 45Ni 45Sn 10 ??732 ??156
??Mn 47Ni 40Sn 13 ??968 ??174
??Mn 50Ni 40Sn 10 ??1231 ??231
??Mn 55Ni 36Sn 9 ??1467 ??303
??Mn 30Ni 48Sn 12 ??175 ??110
It is to be noted and any distortion of making according to the specific embodiment of the present invention all do not break away from the scope that spirit of the present invention and claim are put down in writing.

Claims (9)

1. magnetic material with exchange bias effect, its chemical formula is: Mn mNi nSn oWherein, 30≤m＜55,25≤n≤50,9≤o＜13, m+n+o=100, m, n, o represent atom percentage content.
2. the magnetic material with exchange bias effect as claimed in claim 1 is characterized in that, described Mn mNi nSn oThe form of magnetic material is a mono-crystalline structures.
3. the magnetic material with exchange bias effect as claimed in claim 1 is characterized in that, described Mn mNi nSn oThe form of magnetic material is a polycrystalline structure.
4. one kind prepares claim 1 or 2 arbitrary described methods with magnetic material of exchange bias effect, comprises the steps:
(1) presses chemical formula Mn mNi nSn oRaw materials weighing, wherein, 30≤m＜55,25≤n≤50,9≤o＜13, m+n+o=100, m, n, o represent atom percentage content;
(2) material that will weigh up is contained in the crucible, adopts conventional Czochralski grown Mn mNi nSn oMagnetic mono crystal, its growth conditions is: the heating mentioned component former expect make it fusion; Its fusion environment is 1 * 10 -2To 5 * 10 -5The argon shield gas of the vacuum of Pa or 0.01～1MPa normal pressure; A seed crystal is fixed in seed rod lower end with 0.5～50 rev/min speed rotation; Described seed crystal is a composition monocrystalline identical or approaching, that have needed orientation;
(3) under 1000～1200 ℃ melt temperature condition, kept 10～30 minutes, liquid level with end in contact melt under the seed crystal, with 3～80mm/ hour uniform rate lifting seed rod, lift on the single crystal direction with solidification and crystallization then, and make the single crystal diameter of growth become big or keep certain;
(4) when the monocrystalline of growth reaches required size, single crystal pulling is broken away from the raw material surface of fusion, slowly reduce temperature with 0.5～20 ℃/minute rate of temperature fall and be cooled to room temperature, take out at last.
5. method as claimed in claim 5 is characterized in that, the growth mode of heating in the described step (2) adopts the radio frequency heating or the resistance heating mode of 50～245 KHz.
6. method as claimed in claim 5 is characterized in that, the crucible in the described step (2) is magnetic levitation cold crucible, graphite crucible or silica crucible.
7. method as claimed in claim 5 is characterized in that, the monocrystalline that step (4) prepares was annealed in 500～1200 ℃ temperature range 0.01～100 hour, and then cool off with 0.01～1000 ℃/second rate of temperature fall.
8. one kind prepares claim 1 or 3 arbitrary described methods with magnetic material of exchange bias effect, comprises the steps:
(1) presses chemical formula Mn mNi nSn oRaw materials weighing, wherein, 30≤m＜55,25≤n≤50,9≤o＜13, m+n+o=100, m, n, o represent atom percentage content;
(2) material that will weigh up is contained in the melting kettle, adopts the electric arc melting method to obtain Mn mNi nSn oThe magnetic polycrystalline, its melting condition is: reach 2 * 10 in vacuum -3When Pa is following, feed 0.1～1.2MPa argon gas, whole fusion process sample adopts argon shield, melting electric current 30～100A, and congruent melting refining four times is even to guarantee composition; After the smelted product that is obtained wraps up with tantalum piece, pack in the vitreosil pipe that seals, in 500～1200 ℃ temperature range, annealed 0.1～100 hour, and then cool off with 0.01～1000 ℃/second rate of temperature fall, arrange taking-up at last to realize the atom high-sequential.
9. one kind prepares claim 1 or 3 arbitrary described methods with magnetic material of exchange bias effect, comprises the steps:
To put into the quartz ampoule that gets rid of the band machine as the alloy that obtains at last in claim 8 step (2), be evacuated down to 10 -3More than the Pa, feed high-purity argon gas in the furnace chamber, pressure is 0.05MPa, adopt induction heating, make alloy be in molten condition, be blown into the high-purity argon gas that pressure is 0.1～1.2MPa then from quartz ampoule top, molten alloy liquid is ejected into from aperture on the copper wheel of high speed rotating that linear velocity is 10～30m/s throws away fast, adopting this fast quenching to get rid of band method acquisition width is 1-10mm, and thickness is the polycrystalline state alloy material of 40-50 μ m.
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102751063A (en) * 2012-07-20 2012-10-24 河北师范大学 Magnetic belt material with zero field cooling exchange bias effect and method for preparing magnetic belt material
CN102881393A (en) * 2012-09-11 2013-01-16 华南理工大学 MnFePSi-based room-temperature magnetic refrigeration material and preparation method thereof
CN103334043A (en) * 2013-03-22 2013-10-02 中国科学院物理研究所 Magnetic alloy serving as magnetic refrigeration material
CN103849926A (en) * 2014-03-28 2014-06-11 四川材料与工艺研究所 Method and equipment for pulling high-activity metal monocrystalline
CN106917030A (en) * 2017-04-21 2017-07-04 太原科技大学 A kind of downfield drives orientation Mn Ni Sn magnetic refrigeration alloy material and its method for preparing thin strip thereof
CN108085547A (en) * 2017-12-15 2018-05-29 东北大学 Magnetic material with unusual coercive force temperature coefficient and magnetic refrigerant capacity and preparation method thereof
CN108277406A (en) * 2018-03-19 2018-07-13 河北工业大学 A kind of preparation method of the marmem with exchange bias effect
CN109321792A (en) * 2018-11-20 2019-02-12 西安交通大学 A kind of Mn-Ni-Ga Haas Le alloy material and preparation method thereof with exchange bias effect
CN109576530A (en) * 2018-12-27 2019-04-05 江西理工大学 Huge exchange biased Mn based alloy of one kind and its preparation method and application
CN109873077A (en) * 2019-02-01 2019-06-11 华北电力大学 The method for adjusting the exchange bias field of intermetallic compound
CN115044981A (en) * 2022-06-15 2022-09-13 上海大学 Preparation method and application of antiferromagnetic single crystal material with exchange bias effect
CN115506023A (en) * 2022-09-28 2022-12-23 中国科学院物理研究所 Crystal and preparation method and application thereof

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CN102751063A (en) * 2012-07-20 2012-10-24 河北师范大学 Magnetic belt material with zero field cooling exchange bias effect and method for preparing magnetic belt material
CN102881393A (en) * 2012-09-11 2013-01-16 华南理工大学 MnFePSi-based room-temperature magnetic refrigeration material and preparation method thereof
CN103334043A (en) * 2013-03-22 2013-10-02 中国科学院物理研究所 Magnetic alloy serving as magnetic refrigeration material
CN103334043B (en) * 2013-03-22 2015-07-08 中国科学院物理研究所 Magnetic alloy serving as magnetic refrigeration material
CN103849926A (en) * 2014-03-28 2014-06-11 四川材料与工艺研究所 Method and equipment for pulling high-activity metal monocrystalline
CN106917030B (en) * 2017-04-21 2018-08-28 太原科技大学 A kind of driving of downfield is orientated Mn-Ni-Sn magnetic refrigeration alloy material and its method for preparing thin strip thereof
CN106917030A (en) * 2017-04-21 2017-07-04 太原科技大学 A kind of downfield drives orientation Mn Ni Sn magnetic refrigeration alloy material and its method for preparing thin strip thereof
CN108085547A (en) * 2017-12-15 2018-05-29 东北大学 Magnetic material with unusual coercive force temperature coefficient and magnetic refrigerant capacity and preparation method thereof
CN108085547B (en) * 2017-12-15 2019-12-13 东北大学 Magnetic material with abnormal coercive force temperature coefficient and magnetic refrigeration capability and preparation method thereof
CN108277406A (en) * 2018-03-19 2018-07-13 河北工业大学 A kind of preparation method of the marmem with exchange bias effect
CN109321792A (en) * 2018-11-20 2019-02-12 西安交通大学 A kind of Mn-Ni-Ga Haas Le alloy material and preparation method thereof with exchange bias effect
CN109576530A (en) * 2018-12-27 2019-04-05 江西理工大学 Huge exchange biased Mn based alloy of one kind and its preparation method and application
CN109873077A (en) * 2019-02-01 2019-06-11 华北电力大学 The method for adjusting the exchange bias field of intermetallic compound
CN115044981A (en) * 2022-06-15 2022-09-13 上海大学 Preparation method and application of antiferromagnetic single crystal material with exchange bias effect
CN115044981B (en) * 2022-06-15 2024-03-12 上海大学 Preparation method and application of antiferromagnetic single crystal material with exchange bias effect
CN115506023A (en) * 2022-09-28 2022-12-23 中国科学院物理研究所 Crystal and preparation method and application thereof

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Application publication date: 20100908