CN102751063A - Magnetic belt material with zero field cooling exchange bias effect and method for preparing magnetic belt material - Google Patents
Magnetic belt material with zero field cooling exchange bias effect and method for preparing magnetic belt material Download PDFInfo
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- CN102751063A CN102751063A CN2012102540363A CN201210254036A CN102751063A CN 102751063 A CN102751063 A CN 102751063A CN 2012102540363 A CN2012102540363 A CN 2012102540363A CN 201210254036 A CN201210254036 A CN 201210254036A CN 102751063 A CN102751063 A CN 102751063A
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Abstract
The invention discloses a magnetic belt material with a zero field cooling exchange bias effect. The chemical formula is Mn50CoNi49-xAlx, wherein x which refers to atomic percent content is larger than or equal to 10 and smaller than or equal to 15. The preparation method includes the steps: (1) weighing raw materials according to the chemical formula of Mn50CoNi49-xAlx; (2) containing the raw materials in a water cooling copper crucible, and preparing Mn50CoNi49-xAlx magnetic polycrystalline by means of the conventional electric arc melting method; and (3) using the smelted polycrystalline ingots to prepare the Mn50CoNi49-xAlx magnetic material by means of the rapid quenching method. Compared with existing alloy, the magnetic belt material has the advantages that the exchange bias effect under zero field cooling is achieved, and the magnetic belt material has higher magnetic field controllability, is low in cost and can be used for manufacturing of ultrahigh-density magnetic recording media, magnetic reading heads, giant magnetic resistors, spin valves, novel tunnel junction memories, sensors and the like.
Description
Technical field
The present invention relates to a kind of magnetic material, particularly a kind of Mn with null field cooling exchange bias effect
50CoNi
49-xΛ l
xMagnetic band and preparation method thereof belongs to Material Physics technology category.
Background technology
1956, Meikleijohn and Bean observed exchange biased phenomenon first in Co (ferromagnetic material) particle system that CoO (antiferromagnet) shell covers.When system added the N of magnetic field through 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, is referred to as exchange bias effect to this phenomenon at that time.Its physical mechanism is following: the N T that is in antiferromagnet when system temperature
NCurie temperature T with ferromagnetic material
C(T
N＜T＜T
C) between the time, ferromagnet is in ordered magnetic state in the system, its magnetic moment forwards the direction that is parallel to the outfield under the action of a magnetic field; And antiferromagnet is in paramagnetic state at this moment, and its inner magnetic moment is a disorder distribution.When system is cooled to N when following under magnetic field, at this moment antiferromagnet also gets into 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 let 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 is difficult to overturn, 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, demonstrate unidirectional anisotropy along the cooling field.
At present, in ferromagnetic/antiferromagnetic system that the researcher has been found that exchange biased phenomenon extensively is present in, its
The material of fundamental characteristics and ferromagnetic layer and inverse ferric magnetosphere, thickness and structural approach, succession and process conditions are closely related.Since finding this phenomenon, the pinning effect of exchange bias effect is used widely in permanent magnet, VHD magnetic recording media, magnetic reading head, giant magnetoresistance, Spin Valve, the novel memory of tunnel junction and transducer.Therefore, exchange biased research receives people's attention day by day.
(Z=In, Sn Sb) also have exchange bias effect in the ferromagnetic shape memory alloys material, and for example: people such as Mahmud Khan have reported Ni at Applied PhysicsLetters (91 volumes, 072510 page, 2007) at the NiMnZ of rich Mn in researcher's discovery recently
50Mn
25+xSb
25-xIt is H that sample is observed maximum exchange bias field through cooling (H=5T) under the outside magnetic field
E=248Oe, blocking temperature T
B=115K (T＞T
BThe time, the exchange bias effect of material disappears).2011, people such as L.Ma delivered autograph " Coexistence of reentrant-spin-glass the Mn on Applied Physics Letters
2Ni
1.6Sn
0.4Heusler alloy " article with the H of ferromagnetic shape memory alloys
EBring up to 1100Oe.Though the exchange bias field of material increases, at present traditional have exchange biased magnetic material and must just can show exchange bias effect through a band cooling, and this process has brought inconvenience for the application of material.2011; People such as B.M.Wang deliver the article of autograph for " Large Exchange Bias after Zero-Field Cooling from an Unmagnetized State " on Physical Review Letters; The Ni-Mn-In alloy of having reported the unmagnetized attitude also has big exchange bias effect in the condition of null field cooling, and its exchange bias field is up to 1300 Oe.But consider that major element indium (In) costs an arm and a leg, and is unfavorable for the industrial applications of material.For this reason, research and development have the magnetic material of exchange bias effect under the condition of null field (H=0 Oe) cooling, significant.
Summary of the invention
The purpose of this invention is to provide a kind of magnetic band with null field cooling exchange bias effect.
The present invention also aims to provide a kind of preparation method with magnetic band of null field cooling exchange bias effect.
The objective of the invention is to realize like this: a kind of magnetic band with null field cooling exchange bias effect, its chemical formula is: Mn
50CoNi
49-xAl
x, in the formula, 10≤x≤15, x representes atom percentage content.
The present invention propose like chemical formula Mn
60CoNi
49-xAl
x, the preparation method with magnetic band of null field cooling exchange bias effect comprises the steps:
(1) weighing proportioning
Press chemical formula Mn
50CoNi
49-xAl
xAtomic percent to take by weighing purity be that 99.9% manganese (Mn), purity are that 99.9% cobalt (Co), purity are that 99.9% nickel (Ni) and purity are 99.99% aluminium (Al) bulk;
(2) melting ingot
With the material mixing that weighs up and be contained in the melting kettle, adopt conventional electric arc melting method to obtain Mn
50CoNi
49-xAl
xPolycrystalline, its melting condition is: reach 2 * 10 at base vacuum
-3During Pa, feed argon gas, the argon shield of whole fusion process samples using, melting electric current 100A, each sample upset three times, congruent melting refining four times, even to guarantee composition, finally obtain Mn
50CoNi
49-xAl
xThe magnetic alloy ingot;
(3) fast quenching gets rid of band
The magnetic alloy ingot of suitable size is put into an end opening, other end sealing, sealed end has in the quartz ampoule of aperture, quartz ampoule is placed to gets rid of in the band machine furnace chamber, is evacuated down to 10
-3Below the Pa; Feed high-purity argon gas in the furnace chamber; Make melting furnace chamber internal pressure reach 0.05MPa, adopt induction heating, make alloy be in molten condition; Be blown into high-purity argon gas then from quartz ampoule top and molten alloy liquid be ejected on the copper wheel of high speed rotating that linear velocity is 17m/s throw away fast from aperture, obtaining width is that 3-4mm, thickness are the magnetic band with null field cooling exchange bias effect of 40-50 μ m.
The beneficial effect that the present invention obtains is: the present invention is effective and ingenious to be utilized melting and gets rid of the technology that band combines and prepared Mn
50CoNi
49-xAl
xThe magnetic band, this method has effectively overcome Mn
50CoNi
49-xAl
xSingle-phase not only having a band cooling but also have the magnetic band that null field cools off exchange bias effect prepared in the generation of dephasign in the magnetic material.Magnetic band with exchange bias effect provided by the invention, it shows the characteristic value exchange bias field H that exchange bias effect is renderd a service
ECan be changed or adjust through change Ni, Al ratio of components according to purposes.Therefore, this material has potential use widely, for example magnetic reading head, giant magnetoresistance, Spin Valve, the novel memory of tunnel junction and transducer etc.Prices such as the raw material manganese that the present invention uses, cobalt, nickel, aluminium are cheap, are easy to deposit; Device therefor adds that for the melting of routine fast quenching gets rid of band and do not need
Add miscellaneous equipment; Said material does not need long Ageing Treatment simultaneously, can obtain the sample that performance meets the demands; Therefore, produce Mn
50CoNi
50-xAl
xThe magnetic band is with low cost, and preparation technology is simple, and these characteristics are very beneficial for the batch process and the extensive use of material.
Description of drawings
Accompanying drawing 1:Mn
50CoNi
37Al
12Sample under null field cooling, the M-H curve chart during temperature T=5K.
Accompanying drawing 2:Mn
50CoNi
36Al
13Sample under null field cooling, the M-H curve chart during temperature T=4K.
Accompanying drawing 3:Mn
50CoNi
35Al
14Sample under null field cooling, the M-H curve chart of measurement field H=2T, 4T, 6T during temperature T=4K.
Accompanying drawing 4:Mn
50CoNi
34Al
15Sample under null field cooling, the M-H curve chart during temperature T=4K.
Embodiment
Following embodiment is used to explain the present invention.
(1) weighing proportioning
Press chemical formula Mn
50CoNi
39Al
10Atomic percent to take by weighing purity be that 99.9% manganese (Mn), purity are that 99.9% cobalt (Co), purity are that 99.9% nickel (Ni) and purity are 99.9% aluminium (Al).
(2) melting ingot
The above-mentioned Mn that weighs up, Co, Ni, Al bulk are placed in the melting kettle, with mechanical pump forvacuum to 5 * 10
-1Pa; Be evacuated down to 1 * 10 with molecular pump
-4Pa feeds high-purity argon gas, makes melting chamber internal pressure reach 0.1MPa; Produce electric arc, melting electric current 100A, electric arc head remain on 2-5cm place, sample top and swing 1min repeatedly among a small circle; 3 congruent meltings refining 4 times of overturning so repeatedly of each sample is so that the preparation sample composition is even; Treat that furnace chamber is cooled to room temperature, take out at last.
(3) fast quenching gets rid of band
A part of electric arc melting ingot is put into an end opening, other end sealing, sealed end has in the quartz ampoule of aperture, quartz ampoule is placed to gets rid of in the band machine furnace chamber; Be evacuated down to 10
-3Below the Pa, feed high-purity argon gas in the furnace chamber, pressure is 0.05MPa; 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 from quartz ampoule top and molten alloy liquid be ejected on the copper wheel of high speed rotating that linear velocity is 17m/s throw away fast from aperture.
Under physical property integrated test system (PPMS) measuring samples null field cooling condition, temperature T=4K, the M-H curve chart of different maximum external magnetic field H=2T, 4T, 6T finds that the magnetic hysteresis loop of sample squints, and has exchange bias effect, has exchange bias field H
EWith coercive force H
CAnd the size of its numerical value changes with the variation of external magnetic field, and concrete data are seen chart 1.H wherein
C=| H
L-H
R|/2, H
E=| H
L+ H
R|/2, H
LBe the intersection point on the left side of magnetic hysteresis loop and abscissa, H
RIntersection point for the right of magnetic hysteresis loop and abscissa.
Embodiment 2 preparations consist of Mn
50CoNi
37Al
12Magnetic alloy band with null field cooling exchange bias effect
(1) weighing proportioning
Press chemical formula Mn
50CoNi
37Al
12Atomic percent to take by weighing purity be that 99.9% manganese (Mn), purity are that 99.9% cobalt (Co), purity are that 99.9% nickel (Ni) and purity are 99.9% aluminium (Al).
(2) melting nail material
The above-mentioned Mn that weighs up, Co, Ni, Al bulk are placed in the melting kettle, with mechanical pump forvacuum to 5 * 10
-1Pa; Be evacuated down to 1 * 10 with molecular pump
-4Pa feeds high-purity argon gas, makes melting chamber internal pressure reach 0.1MPa; Produce electric arc, melting electric current 100A, electric arc head remain on 2-5cm place, sample top and swing 1min repeatedly among a small circle; 3 meltings 4 times of overturning so repeatedly of each sample are so that the preparation sample composition is even; Treat that furnace chamber is cooled to room temperature, take out at last.
(3) fast quenching gets rid of band
A part of electric arc melting ingot is put into an end opening, other end sealing, sealed end has in the quartz ampoule of aperture, quartz ampoule is placed to gets rid of in the band machine furnace chamber; Be evacuated down to 10
-3Below the Pa, feed high-purity argon gas in the furnace chamber, pressure is 0.05MPa; 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 from quartz ampoule top and molten alloy liquid be ejected on the copper wheel of high speed rotating that linear velocity is 17m/s throw away fast from aperture.
With physical property integrated test system (PPMS) measuring samples; Measured sample under the null field cooling, external magnetic field H=9T, the M-H curve chart (as shown in Figure 1) of temperature T=5K; The initial magnetic moment of from figure, finding out sample is zero, and the illustrative material initial magnetic state is a magnetic virgin state; The M-H magnetic hysteresis loop squints to initial magnetization direction (positive direction of principal axis), and exchange bias effect is obvious, and the abscissa of M-H closed curve and reference axis intersection point is respectively: H
L=-6238 Oe, H
R=10980Oe obtains coercive force H
CBe 8609Oe, its exchange bias field H
EUp to 2371Oe.
Embodiment 3 preparations consist of Mn
50CoNi
36Al
13The magnetic alloy band with null field cooling exchange bias effect
Its preparation method is with embodiment 2; And measured sample under the null field cooling condition with physical property integrated test system (PPMS); The M-H curve chart (as shown in Figure 2) of temperature T=4K and external magnetic field H=9T; The magnetic hysteresis loop of finding sample squints, and has exchange bias effect, and the abscissa of M-H closed curve and reference axis intersection point is respectively: H
L=-6451.8Oe, H
R=4344.6Oe obtains exchange bias field H
E(H
E=1053.6Oe) with coercive force H
C(H
C=5398.2Oe).Embodiment 4 preparations consist of Mn
50CoNi
35Al
14The magnetic with null field cooling exchange bias effect close
The gold ribbon material
Its preparation method is with embodiment 2, and measured null field cooling sample at temperature T=4K with physical property integrated test system (PPMS), different external magnetic field H=2T, and the M-H curve chart 4T, 6T under, the skew (see figure 3) has taken place in the discovery magnetic hysteresis loop, and Mn is described
50CoNi
35Al
14Sample has exchange bias effect, and exchange bias field and coercive force change with the variation in outfield, and concrete data are seen table 1.
Table 1:Mn
50CoNi
39Al
10And Mn
50CoNi
35Al
41Sample under the null field cooling condition, the H that different external magnetic field H measure during temperature T=4K
EAnd H
CData.
Table 1
Its preparation method is with embodiment 2; And with physical property integrated test system (PPMS) measure null field cooling sample in the outfield H=9T; The M-H curve chart (as shown in Figure 4) of temperature T=4K, the initial magnetic moment of from figure, finding out sample is zero, the illustrative material initial magnetic state is a magnetic virgin state; The M-H magnetic hysteresis loop squints to initial magnetization direction (negative direction of principal axis), and exchange bias effect is obvious, and the abscissa of M-H closed curve and reference axis intersection point is respectively: H
L=-4706Oe, H
R=3393Oe obtains coercive force H
CBe 4049.5Oe, its exchange bias field H
EBe 656.5Oe.
Claims (2)
1. the magnetic band with null field cooling exchange bias effect is characterized in that its chemical formula is: Mn
50CoNi
49-xAl
x, in the formula, 10≤x≤15, x representes atom percentage content.
2. preparation method who prepares the magnetic band that has null field cooling exchange bias effect according to claim 1 is characterized in that may further comprise the steps:
(1) weighing proportioning
Press chemical formula Mn
50CoNi
49-xAl
xAtomic percent to take by weighing purity be that 99.9% manganese (Mn), purity are that 99.9% cobalt (Co), purity are that 99.9% nickel (Ni) and purity are 99.99% aluminium (Al) bulk;
(2) melting ingot
With the material mixing that weighs up and be contained in the melting kettle, adopt conventional electric arc melting method to obtain Mn
50CoNi
49-xAl
xPolycrystalline, its melting condition is: reach 2 * 10 at base vacuum
-3During Pa, feed argon gas, the argon shield of whole fusion process samples using, melting electric current 100A, each sample upset three times, congruent melting refining four times obtains Mn
50CoNi
49-xAl
xThe magnetic alloy ingot;
(3) fast quenching gets rid of band
The magnetic alloy ingot of suitable size is put into an end opening, other end sealing, sealed end has in the quartz ampoule of aperture, quartz ampoule is placed to gets rid of in the band machine furnace chamber, is evacuated down to 10
-3Below the Pa; Feed high-purity argon gas in the furnace chamber; Make melting chamber internal pressure reach 0.05MPa, adopt induction heating, make alloy be in molten condition; Be blown into high-purity argon gas then from quartz ampoule top and molten alloy liquid be ejected on the copper wheel of high speed rotating that linear velocity is 17m/s throw away fast from aperture, obtaining width is that 3-4mm, thickness are the magnetic band with null field cooling exchange bias effect of 40-50 μ m.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981397A (en) * | 2014-05-12 | 2014-08-13 | 太原理工大学 | Ni-Fe-Mn-Al alloy material 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 |
| 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 |
| CN110073448A (en) * | 2016-10-07 | 2019-07-30 | 明尼苏达大学董事会 | Iron-based nano particle and crystal grain |
| 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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| CN101826385A (en) * | 2010-04-30 | 2010-09-08 | 中国科学院物理研究所 | Magnetic material with exchange bias effect and preparation method thereof |
| CN102011038A (en) * | 2010-12-15 | 2011-04-13 | 河北师范大学 | Mn50Ni50-xAlx high-temperature ferromagnetic shape memory alloy material and preparation method thereof |
| CN102115914A (en) * | 2010-12-15 | 2011-07-06 | 河北师范大学 | Mn50CoxNiySnz high-temperature ferromagnetic shape memory alloy material and preparation methods thereof |
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2012
- 2012-07-20 CN CN2012102540363A patent/CN102751063A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101826385A (en) * | 2010-04-30 | 2010-09-08 | 中国科学院物理研究所 | Magnetic material with exchange bias effect and preparation method thereof |
| CN102011038A (en) * | 2010-12-15 | 2011-04-13 | 河北师范大学 | Mn50Ni50-xAlx high-temperature ferromagnetic shape memory alloy material and preparation method thereof |
| CN102115914A (en) * | 2010-12-15 | 2011-07-06 | 河北师范大学 | Mn50CoxNiySnz high-temperature ferromagnetic shape memory alloy material and preparation methods thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981397A (en) * | 2014-05-12 | 2014-08-13 | 太原理工大学 | Ni-Fe-Mn-Al alloy material and preparation method thereof |
| CN103981397B (en) * | 2014-05-12 | 2016-05-11 | 太原理工大学 | A kind of Ni-Fe-Mn-Al alloy material and preparation method thereof |
| CN110073448A (en) * | 2016-10-07 | 2019-07-30 | 明尼苏达大学董事会 | Iron-based nano particle and crystal grain |
| 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 |
| 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 |
| 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: 20121024 |