CN109321792A - A kind of Mn-Ni-Ga Haas Le alloy material and preparation method thereof with exchange bias effect - Google Patents

A kind of Mn-Ni-Ga Haas Le alloy material and preparation method thereof with exchange bias effect Download PDF

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CN109321792A
CN109321792A CN201811388856.5A CN201811388856A CN109321792A CN 109321792 A CN109321792 A CN 109321792A CN 201811388856 A CN201811388856 A CN 201811388856A CN 109321792 A CN109321792 A CN 109321792A
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haas
alloy material
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exchange bias
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CN109321792B (en
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杨森
张垠
李佳宁
田方华
周超
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Xian Jiaotong University
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C22/00Alloys based on manganese
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
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Abstract

The invention discloses a kind of, and the Mn-Ni-Ga Haas with exchange bias effect strangles alloy material, belongs to field of magnetic material preparation, chemical formula Mn50Ni50‑xGax, wherein the atomic percent of x is 2~14.The Mn-Ni-Ga Haas that the invention also discloses a kind of with exchange bias effect strangles the preparation method of alloy material, comprising the following steps: step 1, according to Mn50Ni50‑xGaxAtomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga;Step 2 is obtained Mn-Ni-Ga Haas and is strangled alloy material sample using electric arc melting or directional solidification method preparation Mn, Ni, Ga;Obtained sample is heat-treated and is tested and characterized by step 3.

Description

A kind of Mn-Ni-Ga Haas Le alloy material and its preparation with exchange bias effect Method
Technical field
The present invention relates to field of magnetic material more particularly to a kind of Mn-Ni-Ga Haas with exchange bias effect to strangle and close Golden material and preparation method thereof.
Background technique
1956, Meiklejohn and Bean found in the cobalt cobalt black micro mist with nucleocapsid structure due to it is ferromagnetic/ Antiferromagnetic coupling and the exchange biased phenomenon generated.It is generally acknowledged that exchange bias effect originating from ferromagnetic (FM) with it is antiferromagnetic (AFM) exchange-coupling interaction at interface.When not having outfield, the magnetic moment of inverse ferric magnetosphere is arranged in a jumble.When temperature is reduced to anti-iron When below magnetic Ne&1&el temperature, inverse ferric magnetosphere magnetic moment ordered arrangement.Outside difference off field, the anisotropy of inverse ferric magnetosphere is larger, and Do not change with outfield, but ferromagnetic layer can overturn with outfield and be inverted.Interface inverse ferric magnetosphere can generate interface ferromagnetic layer Pinning effect, so that the magnetic moment of ferromagnetic layer must overcome this pinning effect and could invert.This pinning effect has single To anisotropy, so that ferromagnetic layer is become asymmetric in reversion process, shows as offset of macroscopical hysteresis loop relative to null field, Generate exchange bias effect.Exchange bias field can pass through the intersection point H of hysteresis loop and magnetic field axisL, HRIt is calculated, calculates public Formula is as follows: HE=-(HL+HR)/2。
Exchange bias effect is the basis of information storage technology, is exchanged based on ferromagnetic (FM) and antiferromagnetic (AFM) duplicature The high density playback head of bias effect has high sensitivity, the discovery of the spin valve effect based on exchange bias effect so that Having for giant magnetic resistance substantially develops.Exchange bias effect is widely used in magnetic read head, magnetic random memory and magnetosensitive The fields such as sensor.The development that the research of material in relation to big exchange bias field stores information plays an important roll.
Those skilled in the art is dedicated to developing a kind of new Mn-Ni-Ga Haas Le with big exchange bias effect Alloy material and preparation method, so that Mn-Ni-Ga Haas strangles alloy material and has more wide application potential, to be used for Such as magnetic head, giant magnetoresistance, Spin Valve, tunnel Jie's novel memory devices and sensor etc., to meet the needs of market.
Summary of the invention
In view of the above drawbacks of the prior art, technical problem to be solved by the invention is to provide one kind to have exchange inclined The Mn-Ni-Ga Haas for setting effect strangles alloy material and preparation method, can by change the alloy material component ratio and The condition of external environment adjusts the exchange bias field of the material, thus the different application that must arrive.
To achieve the above object, the present invention provides a kind of, and the Mn-Ni-Ga Haas with exchange bias effect strangles alloy material Material, the chemical formula of the material are Mn50Ni50-xGax, wherein the atomic percent of x is 2~14.
The present invention also provides a kind of, and the Mn-Ni-Ga Haas with exchange bias effect strangles the preparation method of alloy material, The following steps are included:
Step 1, according to Mn50Ni50-xGaxAtomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga;
Step 2, melting Mn, Ni, Ga obtain Mn-Ni-Ga Haas and strangle alloy material sample;
Obtained sample is heat-treated by step 3.
The present invention also provides a kind of, and the Mn-Ni-Ga Haas with exchange bias effect strangles the preparation method of alloy material, The following steps are included:
Step 1, according to Mn50Ni50-xGaxAtomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga;
Step 2, melting Mn, Ni, Ga obtain Mn-Ni-Ga Haas and strangle alloy material sample;
Step 3, preparation directional solidification Mn-Ni-Ga Haas strangle alloy material.
Further, the purity of Mn, Ni, Ga are 99.95%~99.98% in the step 1.
Further, the step 2 includes:
Step 1 weighed Mn, Ni, Ga are sequentially placed into the copper crucible of non-consumable vacuum arc melting furnace, melting is closed Furnace door is evacuated to 5.0 × 10-3Pa is hereinafter, being passed through argon gas to furnace pressure is 3.5 × 104Pa, then the temperature liter in storehouse At to 1500 DEG C~1600 DEG C melt back 4 times or more so that Haas strangle alloy material sample composition it is uniform.
Further, the purity of the argon gas is not less than 99.9996%.
Further, the step 3 includes: that the Mn-Ni-Ga Haas for obtaining step 2 strangles alloy material sample in 900- Anneal 12-14h at 950 DEG C, then furnace cooling to room temperature.
Further, the step 3 includes:
Step 3.1, by step 2 gained sample rough polishing, cleaning, pincers it is broken after be put into alumina ceramic tube, with sample carrier one The open end of alumina ceramic tube is blocked at end, and the other end passes through square thread under sample carrier and connects with traction device, closes sample bin Door is evacuated to 6 × 10-4Pa closes vacuum evacuation device, and argon gas is filled with into door to -5 × 104Pa;
The position of sample carrier is reduced 12mm by traction device by step 3.2, then sets heating schedule to target temperature Stretching run is carried out after keeping the temperature 5mins after 1680 DEG C;
Step 3.3 sets the rate of extension of stretching run as 5um/s, and stretching time 150mins starts to stretch;
Step 3.4, stretching run starting rear towing device are molten to Ga-In alloy with the velocity pull-down of 5um/s by ceramic tube In liquid, aluminium ceramic tube to be oxidized is submerged to sample by Ga-In alloy solution completely and solidifies completely, and stretching run terminates;
Step 3.5 closes heating power supply, is cooled to room temperature to temperature in sample bin and opens sample bin taking-up aluminium oxide ceramics Pipe is gently broken into pieces, is taken out bar to get to directional solidification Mn-Ni-Ga Haas and is strangled alloy material.
Further, the step 3.2 sets heating schedule according to three phases, specific as follows:
Step 3.2.1, initial temperature is set as 25 DEG C, and heating rate 13.75 DEG C/min, time 20mins are warming up to 300 DEG C heat preservation 5mins;
Step 3.2.2, initial temperature is set as 300 DEG C, and heating rate 25 DEG C/min, time 40mins are warming up to 1300 DEG C heat preservation 5mins;
Step 3.2.3, initial temperature is set as 1300 DEG C, and heating rate is 20 DEG C/min, and time 20mins is warming up to 1700℃。
The present invention has the advantage that compared with prior art
(1) magnetic material provided by the invention with big exchange bias effect, the characteristic value of exchange bias effect That is exchange bias field HECan by adjusting Mn, the component ratio of Ni, Ga and change or adjusted according to the concrete application of the material It is whole;
It (2) can be according to Mn50Ni50-xGaxThe concrete application of material adjusts external testing environment locating for the material, to obtain It obtains and applies required exchange bias field, final obtain applies required sensitivity response;
(3) the magnetic material Mn provided by the present invention with big exchange bias effect50Ni50-xGaxIt is answered with wide With prospect, such as magnetic head, giant magnetoresistance, Spin Valve, tunnel Jie's novel memory devices and sensor etc..
It is further said below with reference to technical effect of the attached drawing to design of the invention, concrete scheme and generation It is bright, to be fully understood from the purpose of the present invention, feature and effect.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of a preferred embodiment of the invention;
Fig. 2 is Mn made from the method for the present invention50Ni44Ga6M-H curve when being cooled to 2K from 2T external magnetic field;
Fig. 3 is Mn made from the method for the present invention50Ni42Ga8M-H curve when being cooled to 2K from 2T external magnetic field;
Fig. 4 is Mn made from the method for the present invention50Ni40Ga10M-H curve when being cooled to 2K from 2T external magnetic field;
Fig. 5 is Mn made from the method for the present invention50Ni40Ga10M-H curve when being cooled to 2K from 1T external magnetic field;
Fig. 6 is the Mn of different component made from the method for the present invention50Ni50-xGaxThe exchange bias field and coercivity of material Ga atom content percentage variation diagram.
Specific embodiment
Multiple preferred embodiments of the invention are introduced below with reference to Figure of description 1 to Fig. 6, keep its technology contents more clear It Chu and is easy to understand.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention is simultaneously The non-embodiment for being only limitted to mention in text.
The present invention provides a kind of, and the Mn-Ni-Ga Haas with exchange bias effect strangles alloy material, and chemical formula is Mn50Ni50-xGax, wherein the atomic percent of x is 2~14.
The present invention also provides 2 kinds with exchange bias effect Mn-Ni-Ga Haas strangle alloy material preparation method, Used Mn, Ni, Ga are solid block in experiment:
Preparation method 1: electric arc melting the preparation method
Specifically, according to Mn50Ni50-xGaxAtomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga, Preferably, the purity of Mn, Ni, Ga are respectively between 99.95%~99.98%.
Step 2, melting Mn, Ni, Ga obtain Mn-Ni-Ga Haas and strangle alloy material sample;
Obtained sample is heat-treated by step 3.
Specifically, step 2 includes:
Step 1 weighed Mn, Ni, Ga are sequentially placed into the copper crucible of non-consumable vacuum arc melting furnace, melting is closed Furnace door is evacuated to 5.0 × 10-3Pa is hereinafter, being passed through high-purity argon gas of the purity not less than 99.9996% to furnace pressure is 3.5 ×104Pa, then temperature rises at 1500 DEG C~1600 DEG C melt back 4 times or more so that Haas strangles alloy material in storehouse Sample composition is uniform, and Mn-Ni-Ga Haas that step 2 obtains then is strangled alloy material sample and is annealed at 900-950 DEG C 12- 14h, then furnace cooling to room temperature are made Mn-Ni-Ga Haas and strangle alloy material.
Preparation method 2: directional solidification the preparation method
Specifically, step 1, according to Mn50Ni50-xGaxAtomic percent weigh respectively purity not less than 99.9% Mn, Ni, Ga, it is preferable that the purity of Mn, Ni, Ga are respectively between 99.95%~99.98%;
Step 2, melting Mn, Ni, Ga obtain Mn-Ni-Ga Haas and strangle alloy material sample;
Step 3, preparation directional solidification Mn-Ni-Ga Haas strangle alloy material.
Wherein, step 1 and the step 1 of step 2 and electric arc melting the preparation method are identical as step 2, the directional solidification of step 3 Mn-Ni-Ga Haas strangles alloy material
Step 3.1, by step 2 gained sample rough polishing, cleaning, pincers it is broken after be put into alumina ceramic tube, with sample carrier one The open end of alumina ceramic tube is blocked at end, and the other end passes through square thread under sample carrier and connects with traction device, closes sample bin Door is evacuated to 6 × 10-4Pa closes vacuum evacuation device, and argon gas is filled with into door to -5 × 104Pa;
The position of sample carrier is reduced 12mm by traction device by step 3.2, then sets heating schedule to target temperature Stretching run is carried out after keeping the temperature 5mins after 1700 DEG C,
Wherein, the heating schedule of setting specifically:
Step 3.2.1, initial temperature is set as 25 DEG C, and heating rate 13.75 DEG C/min, time 20mins are warming up to 300 DEG C heat preservation 5mins;
Step 3.2.2, initial temperature is set as 300 DEG C, and heating rate 25 DEG C/min, time 400mins are warming up to 1300 DEG C heat preservation 5mins;
Step 3.2.3, initial temperature is set as 1300 DEG C, and heating rate is 20 DEG C/min, and time 20mins is warming up to 1700℃;
Step 3.3 sets the rate of extension of stretching run as 5um/s, and stretching time 150mins starts to stretch;
Step 3.4, stretching run starting rear towing device are molten to Ga-In alloy with the velocity pull-down of 5um/s by ceramic tube In liquid, aluminium ceramic tube to be oxidized is submerged to sample by Ga-In alloy solution completely and solidifies completely, and stretching run terminates;
Step 3.5 closes heating power supply, is cooled to room temperature to temperature in sample bin and opens sample bin taking-up aluminium oxide ceramics Pipe is gently broken into pieces, is taken out bar to get to directional solidification Mn-Ni-Ga Haas and is strangled alloy material.
4 embodiments of the invention introduced below, are in conjunction with the embodiments further explained technical solution of the present invention.
1 preparation group of embodiment is divided into Mn50Ni44Ga6Haas with exchange bias effect strangle alloy
Step 1, with according to Mn50Ni44Ga6Atomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga, it is excellent Choosing, purity is between 99.95%~99.98%;
Step 1 weighed Mn, Ni, Ga are sequentially placed into the copper crucible of non-consumable vacuum arc melting furnace by step 2, are closed It closes smelting furnace door and is evacuated to 5.0 × 10-3Pa is hereinafter, be passed through high-purity argon gas of the purity not less than 99.9996% to furnace internal pressure Power is 3.5 × 104Pa, then temperature rises at 1500 DEG C~1600 DEG C melt back 4 times or more so that Haas is strangled in storehouse Alloy material sample composition is uniform, and the Mn-Ni-Ga Haas that step 2 obtains then is strangled alloy material sample and is annealed at 900 DEG C 12, then furnace cooling to room temperature is made Mn-Ni-Ga Haas and strangles alloy material.
Step 3, material made from step 2 is taken intermediate stage wire cutting be diameter 10mm, the halfround bar slice of thickness 2mm or The quality of person's other shapes obtains sample to be tested in the particle of 20mg-50mg.
Step 4 carries out sample test.Specifically, using the MPMS-7 of Quantum Design company of U.S. development and production Type SQUID-VSM magnetometer vacuumizes after sample is packed into reference test bar.Temperature in test stalk is risen into 400K, it is then cold in 2T But off field, 10K is cooled to the rate of temperature fall of 35K/min, 2K is then cooled to the rate of temperature fall of 2K/min.Setting measurement model It encloses for -5T-5T, tests the component hysteresis loop i.e. M-H curve, as shown in Fig. 2, M-H hysteresis loop is sent out along magnetic field negative axis directions , there is exchange biased phenomenon in raw obvious offset.It is computed, HEB=1435Oe.
2 preparation group of embodiment is divided into Mn50Ni42Ga8Haas with exchange bias effect strangle alloy
Using preparation method and experiment condition in the same manner as in Example 1, synthesis group is divided into Mn50Ni42Ga8Have exchange The Haas of bias effect strangles alloy, and using the MPMS-7 type SQUID-VSM of U.S. Quantum Design company development and production Magnetometer vacuumizes after sample is packed into reference test bar.Temperature in test stalk is risen into 400K, it is then cooling off field in 2T, with The rate of temperature fall of 35k/min is cooled to 10K, is then cooled to 2K with the rate of temperature fall of 2K/min.Setting measurement range is -5T- 5T tests the component hysteresis loop i.e. M-H curve, as shown in figure 3, M-H hysteresis loop is obvious inclined along the generation of magnetic field negative axis directions It moves, exchange biased phenomenon occurs.It is computed, HEB=2084Oe.
3 preparation group of embodiment is divided into Mn50Ni40Ga10Haas with exchange bias effect strangle alloy
Using preparation method and experiment condition in the same manner as in Example 1, synthesis group is divided into Mn50Ni42Ga10Have hand over The Haas for changing bias effect strangles alloy, and using the MPMS-7 type SQUID- of U.S. Quantum Design company development and production VSM magnetometer vacuumizes after sample is packed into reference test bar.Temperature in test stalk is risen into 400K, it is then cooling off field in 2T, with The rate of temperature fall of 35k/min is cooled to 10K, is then cooled to 2K with the rate of temperature fall of 2K/min.Setting measurement range is -5T- 5T tests the component hysteresis loop i.e. M-H curve, as shown in figure 4, M-H hysteresis loop is obvious inclined along the generation of magnetic field negative axis directions It moves, exchange biased phenomenon occurs.It is computed, HEB=4819Oe.
4 preparation group of embodiment is divided into Mn50Ni40Ga10Haas with exchange bias effect strangle alloy
Using preparation method and experiment condition in the same manner as in Example 1, synthesis group is divided into Mn50Ni40Ga10Have hand over The Haas for changing bias effect strangles alloy, and using the MPMS-7 type SQUID- of U.S. Quantum Design company development and production VSM magnetometer vacuumizes after sample is packed into reference test bar.Temperature in test stalk is risen into 400K, it is then cooling off field in 1T, with The rate of temperature fall of 35k/min is cooled to 10K, is then cooled to 2K with the rate of temperature fall of 2K/min.Setting measurement range is -5T- 5T tests the component hysteresis loop i.e. M-H curve, as shown in figure 5, M-H hysteresis loop is obvious inclined along the generation of magnetic field negative axis directions It moves, exchange biased phenomenon occurs.It is computed, HEB=5132Oe.
Further, the present invention goes back specific experiment Mn50Ni50-xGaxUnder alloy system difference Ga atomic percent this The exchange biased value that golden system obtains, is listed as follows:
1 Mn of table50Ni50-xGaxThe exchange biased value that this gold system obtains under alloy system difference Ga atomic percent
Ga atomic percentage content x (%) HEB(Oe) HC(Oe)
2 1420.13 2283.15
6 1435.31 2911.09
8 2084.32 6339.06
9 4795.05 6944.28
10 4377.06 6049.49
11 628.09 909.49
12 1358.56 1043.79
14 687.46 860.19
Further, data in above table are depicted as curve graph as shown in FIG. 6, from the figure, it can be seen that through 2T It is cooling to cool down exchange bias field H when low temperature 2K off fieldEBFirst increase with the increase of Ga atomic percentage content, in x=9, That is Mn50Ni41Ga9The exchange bias field of component alloy reaches maximum value HEB=4795.05Oe, then with Ga atomic percentage content Increase, exchange bias field is gradually reduced;Coercivity HCSame changing rule is followed first with the increase of Ga atomic percentage content And increase, in x=9, i.e. Mn50Ni41Ga9The coercivity of component alloy reaches maximum value Hc=6944.28Oe, then with Ga original The increase of sub- percentage composition, coercivity are gradually reduced.
In conclusion the disclosure is able to through each reality since related exchange biasing Flow Field Numerical is larger, coercivity is also larger Applying example realizes the respective material and preparation method thereof with big exchange bias effect.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea Scheme, all should be within the scope of protection determined by the claims.

Claims (9)

1. a kind of Mn-Ni-Ga Haas with exchange bias effect strangles alloy material, the chemical formula of the material is Mn50Ni50- xGax, wherein the atomic percent of x is 2~14.
2. a kind of Mn-Ni-Ga Haas with exchange bias effect strangles the preparation method of alloy material according to claim 1, excellent Choosing, comprising the following steps:
Step 1, according to Mn50Ni50-xGaxAtomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga;
Step 2, melting Mn, Ni, Ga obtain Mn-Ni-Ga Haas and strangle alloy material sample;
Obtained sample is heat-treated by step 3.
3. a kind of Mn-Ni-Ga Haas with exchange bias effect strangles the preparation method of alloy material, packet according to claim 1 Include following steps:
Step 1, according to Mn50Ni50-xGaxAtomic percent weigh respectively purity be not less than 99.9% Mn, Ni, Ga;
Step 2, melting Mn, Ni, Ga obtain Mn-Ni-Ga Haas and strangle alloy material sample;
Step 3, preparation directional solidification Mn-Ni-Ga Haas strangle alloy material.
4. the preparation side that the Mn-Ni-Ga Haas according to claim 2 or 3 with exchange bias effect strangles alloy material Method, the purity of Mn, Ni, Ga are 99.95%~99.98% in the step 1.
5. the preparation side that the Mn-Ni-Ga Haas according to claim 2 or 3 with exchange bias effect strangles alloy material Method, the step 2 include: that step 1 weighed Mn, Ni, Ga are sequentially placed into the copper crucible of non-consumable vacuum arc melting furnace, It closes smelting furnace door and is evacuated to 5.0 × 10-3Pa is hereinafter, being passed through argon gas to furnace pressure is 3.5 × 104Pa, then in storehouse Interior temperature rise at 1500 DEG C~1600 DEG C melt back 4 times or more so that Haas to strangle alloy material sample composition uniform.
6. the Mn-Ni-Ga Haas according to claim 5 with exchange bias effect strangles the preparation method of alloy material, The purity of the argon gas is not less than 99.9996%.
7. the Mn-Ni-Ga Haas according to claim 2 with exchange bias effect strangles the preparation method of alloy material, The step 3 includes: that Mn-Ni-Ga Haas that step 2 obtains is strangled alloy material sample to anneal at 900-950 DEG C 12-14h, Then furnace cooling is to room temperature.
8. the Mn-Ni-Ga Haas according to claim 3 with exchange bias effect strangles the preparation method of alloy material, The step 3 includes:
Step 3.1, by step 2 gained sample rough polishing, cleaning, pincers it is broken after be put into alumina ceramic tube, it is stifled with sample carrier one end The firmly open end of alumina ceramic tube, the other end pass through square thread under sample carrier and connect with traction device, close sample bin door, It is evacuated to 6 × 10-4Pa closes vacuum evacuation device, and argon gas is filled with into storehouse to -5 × 104Pa;
The position of sample carrier is reduced 12mm by the traction device by step 3.2, then sets heating schedule to target temperature Stretching run is carried out after keeping the temperature 5mins after 1700 DEG C;
Step 3.3 sets the rate of extension of stretching run as 5um/s, and stretching time 150mins starts to stretch;
Step 3.4, stretching run starting rear towing device by ceramic tube with the velocity pull-down of 5um/s into Ga-In alloy solution, Aluminium ceramic tube to be oxidized is submerged to sample by Ga-In alloy solution completely and solidifies completely, and stretching run terminates;
Step 3.5 closes heating power supply, and it is light to be cooled to room temperature opening sample bin taking-up alumina ceramic tube to temperature in sample bin Touch it is broken, take out bar to get to directional solidification Mn-Ni-Ga Haas strangle alloy material.
9. the Mn-Ni-Ga Haas according to claim 8 with exchange bias effect strangles the preparation method of alloy material, The step 3.2 is specific as follows according to setting heating schedule:
Step 3.2.1, initial temperature is set as 25 DEG C, and heating rate 13.75 DEG C/min, time 20mins are warming up to 300 DEG C of guarantors Warm 5mins;
Step 3.2.2, initial temperature is set as 300 DEG C, and heating rate 25 DEG C/min, time 40mins are warming up to 1300 DEG C of guarantors Warm 5mins;
Step 3.2.3, initial temperature is set as 1300 DEG C, and heating rate is 20 DEG C/min, and time 20mins is warming up to 1700 ℃。
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Title
JYOTI SHARMA AND K. G. SURESH: "Observation of Large Exchange Bias Effect in Bulk Mn50Ni41Sn9 Heusler Alloy", 《IEEE TRANSACTIONS ON MAGNETICS》 *

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