CN116145008A - Mn with zero field cold exchange bias effect 2-x FeCoNi medium-entropy alloy material and preparation method thereof - Google Patents
Mn with zero field cold exchange bias effect 2-x FeCoNi medium-entropy alloy material and preparation method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 77
- 230000000694 effects Effects 0.000 title claims abstract description 44
- 229910002545 FeCoNi Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 64
- 230000005291 magnetic effect Effects 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract 2
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000012856 weighed raw material Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 1
- 230000008878 coupling Effects 0.000 abstract description 23
- 238000010168 coupling process Methods 0.000 abstract description 23
- 238000005859 coupling reaction Methods 0.000 abstract description 23
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 17
- 230000005290 antiferromagnetic effect Effects 0.000 abstract description 10
- 239000010453 quartz Substances 0.000 abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000005316 antiferromagnetic exchange Effects 0.000 abstract 1
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- 238000001228 spectrum Methods 0.000 description 3
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910003286 Ni-Mn Inorganic materials 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 238000010314 arc-melting process Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The invention discloses a medium entropy alloy material with zero field cold exchange bias effect and a preparation method thereof, wherein the chemical formula of the material is Mn 2‑x FeCoNi, x is more than or equal to 0.2 and less than or equal to 0.4, mn is obtained by repeatedly smelting 2‑x The FeCoNi alloy is then sealed in a vacuum quartz tube and put into a muffle furnace for annealing to obtain the alloy. Mn of the present invention 2‑ x The entropy alloy material in FeCoNi has zero field cold exchange bias effect, the size of ferromagnetic and antiferromagnetic exchange coupling can be controlled by the composition change of Mn (0.2-0.4) to obtain specific antiferromagnetic and ferromagnetic coupling proportion, thus obtaining obvious zero field cold exchange bias field without additional external magnetic field accompanied with cooling process, and the material is used in magnetic memory unit and spin valve deviceThe spintronics field such as the parts has potential application prospect.
Description
Technical Field
The invention relates to a magnetic medium entropy alloy material, in particular to Mn with zero field cold exchange bias effect 2-x An FeCoNi medium entropy alloy material and a preparation method thereof.
Background
The discovery of the exchange bias effect is due to Meiklejohn and beans. Both researchers produced CoO-coated Co particles by electrodeposition in 1956. CoO is antiferromagnetic and Co is ferromagnetic. They found that when the temperature is higher than the Neel temperature (T N ) And less than the Curie temperature (T) C ) In this case, the hysteresis loop is shifted horizontally with a decrease in temperature. In 1999, nogues et al summarized this phenomenon of horizontal shift of the hysteresis loop caused by coupling between antiferromagnetic and ferromagnetic bilayer structures, and named the exchange bias effect. Therefore, in general, the exchange bias effect refers to a field-cooled exchange bias effect, which has attracted a wide range of attention due to its application in magnetic recording technology.
In 2011, wang et al in Ni 50 Mn 37 In 13 It was reported for the first time that under zero field cooling conditions, exchange bias effects up to 1300Oe could be achieved, and this phenomenon of hysteresis loop offset without the need for application of an external magnetic field during cooling was named spontaneous exchange bias effect or zero field cold exchange bias effect. To date, zero field cold exchange bias effects have been observed in Ni-Mn based heusler alloy systems, magnetic exchange bias thin film composite systems, perovskite systems, and spinel oxide systems.
Recently, high-entropy alloys (alloys of five and more elements) have received attention because of their excellent breaking strength, tensile strength, corrosion resistance, wear resistance, electrochemical properties, and magnetic properties. In 2017 Schneewiess et al, a vertical exchange bias effect was first found in CrMnFeCoNi with equal atomic ratio; ling in 2022 and the like deposit a layer of CrMnFeCoNi film on the MgO substrate by a laser-assisted molecular beam epitaxy technology, so as to obtain a spontaneous exchange bias effect. This shows that by regulating the ratio of antiferromagnetic/ferromagnetic coupling, a zero field cold exchange bias effect can be obtained in CrMnFeCoNi high entropy alloys. However, the following problems exist in regulating zero-field cold exchange bias effect in CrMnFeCoNi high-entropy alloy: 1. the high-entropy alloy has high confusion of atomic arrangement, even though the alloy is subjected to heat treatment, the uniformity is poor, local hetero-phase clusters are inevitably present in the alloy, and the intrinsic physical properties of the alloy cannot be obtained in the testing process of magnetism and a crystal structure; 2. the zero-field cold exchange bias effect generated by the film system is too small, and the practical application is limited; 3. the material is prepared by a laser auxiliary molecular beam epitaxy technology, and has low yield and high cost.
Disclosure of Invention
The invention aims to provide Mn with zero-field cold exchange bias effect 2-x An FeCoNi medium entropy alloy and a preparation method thereof.
Mn with zero field cold exchange bias effect 2-x The preparation method of the FeCoNi medium entropy alloy comprises the following steps:
step 1: and (3) batching: according to stoichiometric ratio Mn 2-x FeCoNi (x is more than or equal to 0.2 and less than or equal to 0.4) calculates the mass of each element of Mn, fe, co and Ni, wherein Mn element which is easy to volatilize in the arc melting process is treated according to 5 weight percent of excess, and then is weighed;
step 2: vacuum arc melting: the weighed raw materials are put into a water-cooling auxiliary vacuum arc melting furnace crystallizer, and the pressure in the furnace is reduced to 5 x 10 by using a mechanical pump -3 Pa, charging 0.6atm high-purity argon into the furnace body, and repeatedly smelting for 4 times under the smelting current of 90-110A to obtain Mn 2-x Entropy alloy ingot in FeCoNi.
Step 3: vacuum tube sealing annealing: mn obtained in step 2 2-x After cutting the entropy alloy ingot in FeCoNi, placing the cut entropy alloy ingot into a quartz tube, vacuumizing the quartz tube, and sealing the vacuum quartz tube filled with the alloy ingot by using an oxyacetylene welding gun. Placing the vacuum quartz tube with the alloy ingot sealed into a muffle furnace, annealing for 1h at 800 ℃, and then quenching with cold water to obtain Mn 2-x FeCoNi medium entropy alloy.
Compared with the prior art, the invention has the following advantages:
the zero-field cold exchange bias effect is obtained in the medium-entropy alloy by regulating and controlling the component change on the basis of the high-entropy alloy. The intermediate entropy alloy also inherits the strength and toughness of the high entropy alloy, and the application range of the intermediate entropy alloy in magnetic recording technologies such as spin valves and the like is widened.
The ferromagnetic coupling is enhanced by reducing the Mn content alone to obtain the proper antiferromagnetic/ferromagnetic coupling ratio to obtain zero field cold exchange bias effect.
Mn with zero field cold exchange bias effect is obtained through arc melting, vacuum tube sealing annealing and cold water rapid quenching 2- x The FeCoNi medium entropy alloy material has the advantages of simple process flow, low equipment requirement, low raw material cost and convenient mass production.
Drawings
FIG. 1 is Mn 2-x XRD spectrum (a) and partial magnified view (b) of the entropy alloy in FeCoNi (x= 0,0.2 and 0.3).
FIG. 2 shows Mn in example 1 of the present invention 2-x A field-cold exchange bias effect diagram and a zero-field-cold exchange bias effect diagram of the entropy alloy in FeCoNi (x=0) at a 2K temperature of 5T maximum cyclic magnetic field.
FIG. 3 is Mn in example 2 of the present invention 2-x A field-cold exchange bias effect diagram and a zero-field-cold exchange bias effect diagram of the entropy alloy in FeCoNi (x=0.2) at a 2K temperature of 5T maximum cyclic magnetic field.
FIG. 4 shows Mn in example 3 of the present invention 2-x A field-cold exchange bias effect diagram and a zero-field-cold exchange bias effect diagram of the entropy alloy in FeCoNi (x=0.3) at a 2K temperature of 5T maximum cyclic magnetic field.
FIG. 5 shows Mn in examples 1 to 4 of the present invention 2-x The exchange bias field and coercivity of the entropy alloy after zero field cooling in FeCoNi (x=0, 0.2, 0.3 and 0.4) are dependent on composition change.
FIG. 6 shows Mn in examples 1 to 4 of the present invention 2-x Exchange bias field and coercivity dependence of composition change after cooling of the entropy alloy in FeCoNi (x=0, 0.2, 0.3 and 0.4) in a 1T external magnetic field.
Description of the embodiments
In view of the problems in the high-entropy alloys described above, the present invention first eliminates the effect of Cr element, since Cr atoms provide antiferromagnetic coupling, mn atoms change between antiferromagnetic coupling and ferromagnetic coupling with the change in atomic distanceWhen the influence of Cr element is eliminated, the change of magnetic coupling in the alloy is influenced by Mn alone, so that the regulation and control are convenient, the uniformity of the quaternary medium-entropy alloy is better than that of the penta-high-entropy alloy, and the effect of the block material is larger than that of the film material, so that the alloy is more suitable for practical application. Based on this, the present invention proposes that the catalyst is represented by Mn 2-x The component of Mn element is independently changed in the FeCoNi medium entropy alloy to regulate and control the exchange coupling relation between Mn and Mn, thereby obtaining zero-field cold exchange bias effect.
The basic principle of the invention is as follows: fe. Co and Ni provide ferromagnetic coupling in the alloy, while the coupling of Mn atoms is determined by Mn-Mn atomic spacing. When the Mn-Mn atomic spacing is less than 2.83A, antiferromagnetic coupling is exhibited; when the Mn-Mn atomic spacing is greater than 2.83A, ferromagnetic coupling is exhibited. As the proportion of Mn atoms is reduced, the Mn-Mn distance is increased, the ferromagnetic coupling is enhanced, and the proportion of Fe, co and Ni is correspondingly increased, so that the ferromagnetic coupling is enhanced, and the ferromagnetic coupling in the medium-entropy alloy is enhanced as a whole. The initial magnetization process also allows the alloy to acquire disordered spin-like glass behavior at low temperatures. When the ferromagnetic/spin glass coupling coexist, the specific antiferromagnetic/ferromagnetic coupling ratio enables the zero-field cold exchange bias effect to be regulated and controlled by the invention. The exchange bias effect without additional external field cooling has wide application prospect in novel magnetic devices and magnetic recording technologies.
Mn with zero field cold exchange bias effect 2-x The crystalline structure of the FeCoNi medium entropy alloy is characterized by X-ray diffraction (XRD), and the magnetic performance test is characterized by a Magnetic Property Measurement System (MPMS).
Example 1: mn (Mn) 2-x Preparation of entropy alloy in FeCoNi (x=0) and magnetic property test
Step 1: according to stoichiometric ratio Mn 2-x FeCoNi (x=0) calculates the mass of each element Mn, fe, co and Ni required, wherein Mn element which is liable to volatilize during arc melting is treated in an excess of 5wt%, and then weighed.
Step 2: putting the weighed raw materials into a water-cooling auxiliary vacuum arc melting furnace crystallizer, and using a machineThe mechanical pump reduces the pressure in the cavity to 5 x 10 -3 Pa, then filling 0.6atm high purity argon into the cavity, and repeatedly smelting for 4 times under the current of 90A to obtain Mn 2 Entropy alloy ingot in FeCoNi.
Step 3: mn obtained in step 2 2 After cutting the entropy alloy ingot in FeCoNi, placing the cut entropy alloy ingot into a quartz tube, vacuumizing the quartz tube, and sealing the vacuum quartz tube filled with the alloy ingot by using an oxyacetylene welding gun. Will seal Mn 2 Placing a vacuum quartz tube of the entropy alloy ingot in FeCoNi into a muffle furnace, annealing for 1h at 800 ℃, and then quenching with cold water to obtain Mn with better uniformity 2 FeCoNi medium entropy alloy.
For the Mn obtained 2 XRD microstructure characterization and MPMS magnetic performance characterization are carried out on the FeCoNi medium-entropy alloy, an XRD spectrum of the alloy is shown in figure 1, a hysteresis loop of the alloy is shown in figure 2 under the maximum cyclic magnetic field of 2K temperature 5T after zero field cooling and after 1T external magnetic field cooling, and corresponding exchange bias field and coercivity values are shown in figures 5 and 6.
Example 2: mn (Mn) 2-x Preparation of entropy alloy in FeCoNi (x=0.2) and magnetic property test
The Mn obtained in example 1 was obtained by changing "x=0" in the dosing step of example 1 to "x=0.2" under the same conditions as in example 1 1.8 The XRD microstructure characterization and MPMS magnetic property characterization of the entropy alloy in FeCoNi are respectively carried out, the XRD spectrogram of the alloy is shown in figure 1, the hysteresis loop of the alloy is shown in figure 3 under the maximum cyclic magnetic field of 2K temperature 5T after zero field cooling and after 1T external magnetic field cooling, and the corresponding exchange bias field and coercive force values are shown in figures 5 and 6.
Example 3: mn (Mn) 2-x Preparation of entropy alloy in FeCoNi (x=0.3) and magnetic property test
Other conditions for the preparation were the same as in example 1 except that "x=0" in the dosing section of example 1 was changed to "x=0.3", and the obtained Mn was obtained 1.7 The entropy alloy in FeCoNi is respectively subjected to XRD microstructure characterization and MPMS magnetic property characterization, the XRD spectrum of the alloy is shown in figure 1, the hysteresis loop under the maximum cyclic magnetic field of 2K temperature 5T after zero field cooling and after 1T external magnetic field cooling is shown in figure 4, and the corresponding exchange bias field are shown in the specificationThe coercivity values are shown in fig. 5 and 6.
Example 4: mn (Mn) 2-x Preparation of entropy alloy in FeCoNi (x=0.4) and magnetic property test
The Mn obtained in example 1 was obtained by changing "x=0" in the dosing step of example 1 to "x=0.4" under the same conditions as in example 1 1.7 The entropy alloy in FeCoNi is subjected to MPMS magnetic performance characterization, and corresponding exchange bias field and coercivity values are shown in fig. 5 and 6.
Test results show that after zero field cooling, the alloy can be used for cooling the alloy in Mn 2-x Zero field cold exchange bias effect is obtained in the entropy alloy in FeCoNi (x=0, 0.2, 0.3 and 0.4). As shown in fig. 5 and 6, as the Mn content decreases, the zero-field cold exchange bias field decreases and increases, and an effect peak is obtained when x=0.3, and as the Mn content further decreases, the zero-field cold exchange bias effect decreases, and the field cold exchange bias effect and the coercive force corresponding to the two have the same tendency. As shown in the XRD pattern of fig. 1, this is because during the course of x=0 to x=0.2, the original split peak of x=0 disappears, which indicates that a structural change occurs, resulting in weakening of the ferromagnetic coupling, so that the zero field cold exchange bias effect near vanishes at x=0.2, and the corresponding zero field cold exchange bias field decreases from 0.053kOe at x=0 to 0.0075kOe at x=0.2. And when x=0.3, the maximum zero field cold exchange bias field H is obtained ZEB At 0.415kOe, the corresponding coercive force is 3.385kOe, and after 1T field cooling, the field-cooling exchange bias effect H is obtained under 2K temperature and 5T maximum cyclic magnetic field CEB 3.79kOe, and the corresponding coercivity is 1.75kOe. When x=0.4, the zero-field cold exchange bias field is reduced due to the change of the ratio of ferromagnetic coupling and antiferromagnetic coupling, and the H is reduced ZEB The coercivity was 0.13kOe, with a corresponding coercivity of 0.76kOe.
Claims (6)
1. A medium entropy alloy material with zero field cold exchange bias effect, characterized in that: the chemical formula of the medium entropy alloy material with zero field cold exchange bias effect is Mn 2-x FeCoNi ，0.2≤x≤0.4。
2. The method as claimed in claim 1The medium entropy alloy material is characterized in that: when x=0.3, under 2K conditions, the medium entropy alloy material attains a maximum zero field cold exchange bias field (H) when the maximum circulating magnetic field reaches 5T ZEB ) At 0.415kOe, the corresponding coercivity (H C ) 3.385kOe.
3. A preparation method of a medium entropy alloy material with zero field cold exchange bias effect is characterized by comprising the following steps: the method comprises the following steps:
step 1, batching: according to stoichiometric ratio Mn 2-x FeCoNi, wherein x is more than or equal to 0.2 and less than or equal to 0.4, and the mass of each element of Mn, fe, co and Ni is calculated, wherein the element of Mn which is easy to volatilize is excessively weighed;
step 2, vacuum arc melting: weighing raw materials, and carrying out vacuum arc melting to obtain Mn 2-x Entropy alloy ingot in FeCoNi;
step 3, vacuum tube sealing annealing: mn as described above 2-x Cutting the FeCoNi intermediate entropy alloy ingot, then carrying out vacuum annealing at a certain temperature, and carrying out cold water rapid quenching to obtain the intermediate entropy alloy material.
4. A method as claimed in claim 3, wherein: the volatile Mn element is weighed out in 5% by weight excess.
5. A method as claimed in claim 3, wherein: the weighed raw materials are put into a water-cooling auxiliary vacuum arc melting furnace crystallizer, and the pressure in the furnace is reduced to 5 x 10 -3 Pa, charging 0.6atm high-purity argon into the furnace body, and repeatedly smelting for 4 times under the smelting current of 90-110A to obtain Mn 2-x Entropy alloy ingot in FeCoNi.
6. A method as claimed in claim 3, wherein: vacuum annealing was performed at 800℃for 1h.
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Citations (4)
| 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 |
| KR101910744B1 (en) * | 2017-07-26 | 2018-10-22 | 포항공과대학교 산학협력단 | Medium-entropy alloys with excellent cryogenic properties |
| TWI730685B (en) * | 2020-03-23 | 2021-06-11 | 國立臺灣大學 | A high/medium entropy alloy with hierarchical twin structure |
| CN115505812A (en) * | 2022-09-16 | 2022-12-23 | 华东理工大学 | Soft magnetic medium-entropy alloy and preparation method and application thereof |
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| 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 |
| KR101910744B1 (en) * | 2017-07-26 | 2018-10-22 | 포항공과대학교 산학협력단 | Medium-entropy alloys with excellent cryogenic properties |
| TWI730685B (en) * | 2020-03-23 | 2021-06-11 | 國立臺灣大學 | A high/medium entropy alloy with hierarchical twin structure |
| CN115505812A (en) * | 2022-09-16 | 2022-12-23 | 华东理工大学 | Soft magnetic medium-entropy alloy and preparation method and application thereof |
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