CN109873077B - Method for adjusting exchange bias field of intermetallic compound - Google Patents
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Abstract
The invention discloses a method for adjusting an exchange bias field of an intermetallic compound. The invention provides a method for regulating Mn3Zn1‑xCoxExchange of N intermetallic compoundsA method of biasing a field, comprising the steps of: regulating Mn within the range of x being more than or equal to 0.5 and less than or equal to 0.93Zn1‑xCoxSize of x value of N intermetallic compound, preparation of Mn having different x values3Zn1‑xCoxAn N intermetallic compound; and/or Mn to be produced3Zn1‑xCoxCooling the N intermetallic compound to 5-65K, Mn under the conditions of room temperature and additional 5T magnetic field3Zn1‑xCoxThe N intermetallic compound can generate exchange bias fields of different sizes. In the method disclosed by the invention, when x is 0.9, the exchange bias field reaches 11.02-13.3 kOe rarely in the temperature range of 5K-65K, and the exchange bias field is reduced along with the increase of the temperature in the temperature range, so that the crystal can be applied to the fields of information storage, magnetic field detection, magnetic fingerprint identification and the like, wherein the exchange bias field needs to be adjusted by adjusting the temperature.
Description
Technical Field
The invention relates to the field of magnetoelectronic devices, in particular to a method for adjusting an exchange bias field of an intermetallic compound.
Background
The exchange bias effect is caused by the exchange coupling action at the interfaces of different magnetic phases of the material, and under the driving of the exchange coupling action, the magnetic phenomenon that the hysteresis loop center of the material deviates from the zero point of a magnetic field is an important magnetic phenomenon, and the deviation amount is called an exchange bias field. The exchange bias field is an interface effect, and the magnitude of the exchange bias field is strongly dependent on the interface spin configuration, anisotropy, antiferromagnetic spin orientation, cooling field, interface roughness and other factors. The exchange bias field of the ferromagnetic/antiferromagnetic system has rich physical significance and has important application value in giant magneto-resistance devices. The exchange bias effect is an important foundation of information storage technology and has wide application prospect in a plurality of related fields.
In GMR/TMR spin valve sensors, a device with an exchange bias field is required. In GMR/TMR spin valve sensors, an exchange bias of antiferromagnetic and ferromagnetic layers is used as a pinned layer, and a free layer of ferromagnetic thin film is added. Under the action of an external magnetic field, the magnetic moment of the free layer is parallel to the external magnetic field, but the magnetic moment of the pinned layer needs to be kept constant. If the external magnetic field is too large, the exchange bias field may be exceeded, resulting in a change in the magnetic moment of the pinned layer, rendering the sensor ineffective. To not fail under large magnetic fields, it is generally necessary to increase the bias field to keep the pinned layer magnetic moment stable. The magnitude of the exchange bias field actually determines the maximum operating magnetic field of such sensors. If it is desired to use such sensors in an external field environment of different magnitudes, the magnitude of the switching bias needs to be adjusted.
Anti-perovskite structure Mn3Zn1-xCoxThe N intermetallic compound is a novel compound with many novel physical properties, and the crystal structure is a cubic structure, Mn atoms are positioned at the face center of a unit cell, Zn/Co atoms are positioned at the apex angle, and N atoms are positioned at the body center. The electric transport and thermal expansion behaviors of the compounds are changed along with the transformation of magnetic properties, thereby causing wide attention in academia and industry.
No prior art currently discloses Mn3Zn1-xCoxExchange bias properties of N intermetallics. In the prior art, the size of the switching bias field applied to information storage, spin valve, etc. is mainly focused on the range of 1-2 KOe. In the evolving information storage technology, the requirements for the controllability of the switching bias field are increasing.
Disclosure of Invention
In order to make up for the deficiency of adjusting the exchange bias field in the field, the invention provides a method for adjusting Mn3Zn1-xCoxA method of exchanging bias fields of N intermetallics.
The invention adopts the following technical scheme:
adjustment of Mn3Zn1-xCoxA method of exchanging bias fields for N intermetallics, comprising the steps of: regulating Mn within the range of x being more than or equal to 0.5 and less than or equal to 0.93Zn1-xCoxSize of x value of N intermetallic compound, preparation of Mn having different x values3Zn1-xCoxAn N intermetallic compound; and/or Mn to be produced3Zn1-xCoxCooling the N intermetallic compound to 5-65K, Mn under the conditions of room temperature and additional 5T magnetic field3Zn1-xCoxThe N intermetallic compound can generate exchange bias fields of different sizes.
x represents the content ratio of the Co element at the vertex angle position in the crystal lattice. In the range of x is more than or equal to 0.5 and less than or equal to 0.9, the larger the value of x (namely, the higher the content of Co element), the Mn3Zn1-xCoxThe larger the exchange bias field generated by the N intermetallic compound.
The value of x is more than or equal to 0.5 and less than or equal to 0.9, and the Mn to be prepared3Zn1-xCoxCooling the N intermetallic compound to 5-65K, Mn under the conditions of room temperature and additional 5T magnetic field3Zn1-xCoxThe N intermetallic compound can generate different exchange bias fields in the range of 392 Oe-13.3 KOe.
When x is 0.9, adding Mn3Zn0.1Co0.9The N intermetallic compound powder is cooled to 5K-65K under the conditions of room temperature and an external 5T magnetic field, and the generated exchange bias field ranges from 11.02kOe to 13.3 kOe.
When x is 0.7, adding Mn3Zn0.3Co0.7The N intermetallic compound powder is cooled to 5K-65K under the conditions of room temperature and an external 5T magnetic field, and the generated exchange bias field ranges from 1.27kOe to 6.651 kOe.
When x is 0.5, adding Mn3Zn0.5Co0.5The N intermetallic compound powder is cooled to 5K-65K under the conditions of room temperature and an external 5T magnetic field, and the generated exchange bias field ranges from 392Oe to 975 Oe.
The cooling is liquid helium cooling.
The Mn is3Zn1-xCoxA method for producing an N intermetallic compound, comprising the steps of:
(1)Mn2preparation of N: introducing N into Mn powder2Reacting at 730-780 ℃ to obtain Mn2N；
(2) Mn is weighed according to the molar ratio shown in the formula (1)2Grinding N powder, Zn powder and Co powder to uniformly mix all the powder; the chemical formula of the reaction is:
3Mn2N+2(1-x)Zn+2xCo→2Mn3Zn1-xCoxN+N2(formula 1)
(3) Pressing the powder into a sheet with the thickness of 2-3 mm under the pressure of 20-25 MPa;
(4) the pressed tablets were subjected to a vacuum treatment, when the vacuum reached 10-5～10-6Pa, sealing the reaction container;
(5) heating the closed reaction vessel to 750-820 ℃, preserving the heat for 80-90 hours, and then cooling to room temperature along with the furnace;
(6) mn obtained after cooling3Zn1-xCoxAn N intermetallic compound.
In the step (1), the reaction is carried out at 730-780 ℃ and the temperature is increased to 730-780 ℃ at the rate of 10 ℃ per minute, the temperature is kept for 2700 minutes, and then the furnace is cooled to the room temperature; and the nitrogen flow is kept at 80ml/min all the time in the processes of temperature rising, heat preservation and temperature reduction.
In the step (5), the temperature is raised to 750-820 ℃ at a rate of 10 ℃ per minute.
The grinding time in the step (2) is 45-60 minutes.
In the evolving information storage technology, the requirements for the controllability of the switching bias field are increasing. In the method disclosed by the invention, when x is 0.9, the exchange bias field reaches 11.02-13.3 kOe rarely in the temperature range of 5K-65K, and the exchange bias field is reduced along with the increase of the temperature in the temperature range, so that the crystal can be applied to the fields of information storage, magnetic field detection, magnetic fingerprint identification and the like, wherein the exchange bias field needs to be adjusted by adjusting the temperature.
In another embodiment, when x is 0.7, the exchange bias field ranges from 1.27K to 6.651kOe at a temperature ranging from 5K to 65K, spanning a larger range of exchange bias field sizes up to 5.381 kOe; the crystal produces an exchange bias field whose magnitude varies more significantly with temperature and whose magnitude is also within the applicable range, and may be more suitable for applications where it is desirable to adjust the exchange bias field by adjusting the temperature.
Mn disclosed in the invention3Zn1-xCoxThe N intermetallic compound has larger exchange bias field, so that the use of the N intermetallic compound as the material of the pinning layer in the GMR/TMR spin valve sensor can increase the stability of the sensor and expand the application range, Mn3Zn1- xCoxThe N intermetallic compound powder may be in the form of a pellet or may be doped with other materials as an original of the pinning layer, instead of the existing thin film.
With Mn3Zn1-xCoxThe advantage of the method of generating different size exchange bias field by N intermetallic compound is that:
(1) some existing materials generating exchange bias field have small exchange bias effect, and are difficult to apply to various fields of information storage technology and the like, such as unstable devices, low signal-to-noise ratio and the like, while Mn3Zn1-xCoxN can lead Mn to be generated by selecting the cobalt content and the temperature3Zn1-xCoxThe switching bias field above 5kOe is generated, and the method is suitable for application in various fields such as information storage technology and the like;
(2) when the value of x is not changed, for Mn3Zn1-xCoxThe size of an exchange bias field of the N intermetallic compound can be changed by adjusting the temperature within the range of 5-65K, so that the N intermetallic compound can be respectively as follows: when x is 0.9, the range of the exchange bias field is 11.02-13.3 kOe; when x is 0.7, the range of the exchange bias field is 1.27-6.651 kOe; when x is 0.5, the range of the exchange bias field is 392-975 Oe, and the improvement of the exchange bias field can improve the response sensitivity of the device and reduce the requirement of the application of the device on the environment. If the temperature is reduced to improve the corresponding sensitivity during the preparation process by adopting the material, the device can be used at low temperature if the exchange bias is generated at low temperature.
(3) In addition to exchange bias fields, the Mn disclosed in this application3Zn1-xCoxThe N intermetallic compound also has a vertical offset, and when the temperature is changed within the range of 5-65K, and when x is 0.9, the vertical offset is within the range of 0.027325-0.03093 muBU. d; when x is 0.7, the vertical offset is in the range of 0.00524 to 0.01502 muBF.u; when x is 0.5, the vertical offset is 0.01866-0.024235 muBU. the existence of vertical offset can enrich the design mode of the sensor.
Drawings
FIG. 1 shows Mn3Zn1-xCoxA crystal structure schematic diagram of the N metal compound;
FIG. 2 shows Mn at 5K3Zn0.1Co0.9A hysteresis loop of N;
FIG. 3 shows Mn at 5K3Zn0.3Co0.7A hysteresis loop of N;
FIG. 4 shows Mn at 5K3Zn0.5Co0.5A hysteresis loop of N;
FIG. 5 Mn at 25K3Zn0.1Co0.9A hysteresis loop of N;
FIG. 6 Mn at 25K3Zn0.3Co0.7A hysteresis loop of N;
FIG. 7 Mn at 25K3Zn0.5Co0.5A hysteresis loop of N;
FIG. 8 shows Mn at 45K3Zn0.1Co0.9A hysteresis loop of N;
FIG. 9 shows Mn at 45K3Zn0.3Co0.7A hysteresis loop of N;
FIG. 10 shows Mn at 45K3Zn0.5Co0.5A hysteresis loop of N;
FIG. 11 Mn at 65K3Zn0.1Co0.9A hysteresis loop of N;
FIG. 12 Mn at 65K3Zn0.3Co0.7A hysteresis loop of N;
FIG. 13 Mn at 65K3Zn0.5Co0.5A hysteresis loop of N;
FIG. 14 is a graph of the exchange bias field for three samples at different temperatures.
Detailed Description
Sources of reagents used in the invention: mn powder, Zn powder and Co powder are purchased from Beijing Liyuanxinxin Metal materials science and technology Limited, and the purity is more than or equal to 99.99 percent.
Example 1 Mn3Zn1-xCoxPreparation method and temperature of N and Mn/Zn/Co ratio3Zn1-xCoxInfluence of N exchange bias field
One, Mn3Zn1-xCoxThe preparation method of N comprises the following synthetic steps:
(1) preparation of Mn3Zn1-xCoxThe raw materials of the N intermetallic compound are respectively Mn powder, Zn powder and Co powder with the purity of 99.99 percent;
(2) weighing quantitative Mn powder, putting the Mn powder into a quartz boat, and carrying out nitriding treatment in a chemical vapor deposition furnace; the CVD quartz tube was purged with nitrogen gas having a purity of 99.99% three times, then heated to 730 ℃ at a rate of 10 ℃ per minute, held for 2700 minutes, and then furnace-cooled to room temperature. Keeping the nitrogen flow at 80ml/min all the time in the processes of heating, heat preservation and cooling to obtain Mn2N；
4Mn+N2→2Mn2N
(3) Weighing Mn according to a molar ratio2N powder, Zn powder and Co powder, ground in an agate mortar for 45 minutes to mix all of them uniformly; theThe chemical formula of the reaction is:
3Mn2N+2(1-x)Zn+2xCo→2Mn3Zn1-xCoxN+N2
(4) pressing the powder into a wafer with the diameter of 12mm and the thickness of 2-3 mm by using a grinding tool with the diameter of 12mm under the pressure of 20 Pa;
(5) the pressed wafer is placed in a quartz tube and rapidly connected to a vacuum-pumping system, when the vacuum reaches 10%-5～10-6Pa, then sealing the quartz tube;
(6) heating the sealed quartz tube to 750 ℃ in a high-temperature furnace at the rate of 10 ℃ per minute, preserving the heat for 80-90 hours, then turning off a power supply, and cooling the quartz tube to room temperature along with the furnace;
(7) cooling and taking out the calcined Mn3Zn1-xCoxThe N intermetallic compound is the target product.
Analysis by X-ray diffraction method gave Mn as shown in FIG. 13Zn1-xCoxCrystal structure of N metal compound.
Second, temperature and ratio of Zn to Co to Mn3Zn1-xCoxInfluence of N exchange bias field
This example tests Mn at different temperatures for different Zn-Co ratios3Zn1-xCoxN the magnitude of the generated exchange bias field.
1. Test subjects: mn3Zn1-xCoxAnd (4) N powder. (particle size of powder 5 to 20 μm)
2. The test method comprises the following steps:
the test procedure was as follows:
(1) mn was synthesized according to the method of example 13Zn0.1Co0.9N (sample 1), Mn3Zn0.3Co0.7N (sample 2) and Mn3Zn0.5Co0.5N (sample 3);
(2) respectively measuring field-cooled magnetic hysteresis loops of the powder of the samples 1-3 under the condition of 5T of the combined external magnetic field of 5K, 25K, 45K and 65K by using a SQUID-VSM magnetometer;
(3) the specific measurement process is as follows: the sample powder is cooled to 5K by liquid helium under the condition of room temperature and the condition of an external 5T magnetic field, then the testing instrument starts to add the testing magnetic field from 0 to 7(8) T, then the magnetic field is gradually reduced to 0 and then is reduced to-7 (8) T, the magnetic field is gradually increased to 0, and then the testing is stopped when the magnetic field is increased to 7(8) T.
3. Results of the experiment
(1) The temperature is 5K, and the external magnetic field is 5T
1)Mn3Zn0.1Co0.9N has an exchange bias field size of 13.3KOe and a vertical offset of 0.03093 μBU. d; the hysteresis loop is shown in figure 2; the calculation method of the exchange bias field is HEB＝(HL+HR) /2 wherein HLIs the intersection of the hysteresis loop with the left side of the abscissa, HRIs the intersection point of the hysteresis loop and the right side of the abscissa; the calculation method of the vertical offset is Mshift＝(M++M-) /2 wherein M+For maximum positive magnetization, M-Magnetization in the most negative direction;
2)Mn3Zn0.3Co0.7n has an exchange bias field size of 6.651KOe and a vertical offset of 0.01483 muBU. d; the hysteresis loop is shown in figure 3;
3)Mn3Zn0.5Co0.5n has an exchange bias field size of 975Oe and a vertical offset of 0.01866 muBU. d; the hysteresis loop is shown in figure 4;
(2) the temperature is 25K, and the external magnetic field is 5T
1)Mn3Zn0.1Co0.9N has an exchange bias field size of 12.67KOe and a vertical offset of 0.03093 μBU. d; the hysteresis loop is shown in figure 5; the calculation method of the exchange bias field is HEB＝(HL+HR) /2 wherein HLIs the intersection of the hysteresis loop with the left side of the abscissa, HRIs the intersection point of the hysteresis loop and the right side of the abscissa; the calculation method of the vertical offset is Mshift＝(M++M-) 2; wherein M is+For maximum positive magnetization, M-Maximum negative direction of magnetization；
2)Mn3Zn0.3Co0.7N has an exchange bias field size of 6.20KOe and a vertical offset of 0.01502 μBU. d; the hysteresis loop is shown in figure 6;
3)Mn3Zn0.5Co0.5n has an exchange bias field size of 803Oe and a vertical offset of 0.022355 μBU. d; the hysteresis loop is shown in figure 7;
(3) the temperature is 45K, and the external magnetic field is 5T
1)Mn3Zn0.1Co0.9N has an exchange bias field size of 12.19KOe and a vertical offset of 0.030605 μBU. d; the hysteresis loop is shown in figure 8; the calculation method of the exchange bias field is HEB＝(HL+HR) 2; wherein H isLIs the intersection of the hysteresis loop with the left side of the abscissa, HRIs the intersection point of the hysteresis loop and the right side of the abscissa; the calculation method of the vertical offset is Mshift＝(M++ M-)/2; wherein M is+For maximum positive magnetization, M-Magnetization in the most negative direction;
2)Mn3Zn0.3Co0.7n has a switching bias field size of 4.22KOe and a vertical offset of 0.010805 μBU. d; the hysteresis loop is shown in figure 9;
3)Mn3Zn0.5Co0.5n has a switching bias field size of 637Oe and a vertical offset of 0.024235 μBU. d; the hysteresis loop is shown in figure 10;
(4) the temperature is 65K, and the external magnetic field is 5T
1)Mn3Zn0.1Co0.9N has an exchange bias field size of 11.02KOe and a vertical offset of 0.027325 μBU. d; the hysteresis loop is shown in figure 11; the calculation method of the exchange bias field is HEB＝(HL+HR) /2 wherein HLIs the intersection of the hysteresis loop with the left side of the abscissa, HRIs the intersection point of the hysteresis loop and the right side of the abscissa; the calculation method of the vertical offset is Mshift＝(M++M-) 2; wherein M is+Is maximally positiveDirection magnetization, M-Magnetization in the most negative direction;
2)Mn3Zn0.3Co0.7n has an exchange bias field size of 1.27KOe and a vertical offset of 0.00524 μBU. d; the hysteresis loop is shown in figure 12;
3)Mn3Zn0.5Co0.5n has an exchange bias field size of 392Oe and a vertical offset of 0.020075 μBU. d; the hysteresis loop is shown in figure 13;
from the above results, it can be seen that Mn is present when the temperature is in the range of 5 to 65K and the value of x is in the range of 0.5 to 0.93Zn1- xCoxThe N crystal structure can generate different exchange bias fields in the range of 392 Oe-13.3 KOe, and the vertical offset is 0.05-0.31 muBIn the/f.u. range, the method is suitable for application in various fields such as information storage technology and the like. The relationship of the exchange bias field at different temperatures for the three samples is shown in FIG. 14.
Example 2 Mn3Zn1-xCoxPreparation method and temperature of N and Mn/Zn/Co ratio3Zn1-xCoxInfluence of N exchange bias field
One, Mn3Zn1-xCoxThe preparation method of N comprises the following synthetic steps:
(1) preparation of Mn3Zn1-xCoxThe raw materials of the N intermetallic compound are respectively Mn powder, Zn powder and Co powder with the purity of 99.99 percent;
(2) weighing quantitative Mn powder, putting the Mn powder into a quartz boat, and carrying out nitriding treatment in a chemical vapor deposition furnace; the CVD quartz tube was purged with nitrogen gas having a purity of 99.99% three times, then heated to 780 ℃ at a rate of 10 ℃ per minute, held for 2700 minutes, and then furnace-cooled to room temperature. Keeping the nitrogen flow at 80ml/min all the time in the processes of heating, heat preservation and cooling to obtain Mn2N；
4Mn+N2→2Mn2N
(3) Weighing Mn according to a molar ratio2N powder, Zn powder and Co powder, ground in an agate mortar for 60 minutes to mix all their powders uniformly; the reactionThe chemical formula of (A) is:
3Mn2N+2(1-x)Zn+2xCo→2Mn3Zn1-xCoxN+N2
(4) pressing the powder into a wafer with the diameter of 12mm and the thickness of 2-3 mm by using a grinding tool with the diameter of 12mm under the pressure of 25 Pa;
(5) the pressed wafer is placed in a quartz tube and rapidly connected to a vacuum-pumping system, when the vacuum reaches 10%-5～10-6Pa, then sealing the quartz tube;
(6) heating the sealed quartz tube to 820 ℃ in a high-temperature furnace at the rate of 10 ℃ per minute, preserving the heat for 80-90 hours, then turning off a power supply, and cooling the quartz tube to room temperature along with the furnace;
(7) cooling and taking out the calcined Mn3Zn1-xCoxThe N intermetallic compound is the target product.
The Mn shown in FIG. 1 was also obtained by X-ray diffraction analysis3Zn1-xCoxCrystal structure of N metal compound.
Second, temperature and ratio of Zn to Co to Mn3Zn1-xCoxInfluence of N exchange bias field
This example tests Mn at different temperatures for different Zn-Co ratios3Zn1-xCoxN the magnitude of the generated exchange bias field.
1. Test subjects: mn3Zn1-xCoxAnd (4) N powder. (particle size of powder 5 to 20 μm)
2. The test method comprises the following steps:
same as in example 1.
3. The experimental results are as follows:
there was no significant difference from example 1.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (9)
1. Adjustment of Mn3Zn1-xCoxA method of exchanging bias fields for N intermetallics, comprising the steps of: regulating Mn within the range of x being more than or equal to 0.5 and less than or equal to 0.93Zn1-xCoxSize of x value of N intermetallic compound, preparation of Mn having different x values3Zn1-xCoxAn N intermetallic compound; and/or Mn to be produced3Zn1-xCoxCooling the N intermetallic compound to 5-65K, Mn under the conditions of room temperature and additional 5T magnetic field3Zn1-xCoxThe N intermetallic compound can generate exchange bias fields with different sizes, and x is any value of x which is more than or equal to 0.5 and less than or equal to 0.9;
the value of x is more than or equal to 0.5 and less than or equal to 0.9, and the Mn to be prepared3Zn1-xCoxCooling the N intermetallic compound to 5-65K, Mn under the conditions of room temperature and additional 5T magnetic field3Zn1-xCoxThe N intermetallic compound can generate different exchange bias fields in the range of 392 Oe-13.3 KOe.
2. Regulation Mn according to claim 13Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: when x is 0.9, adding Mn3Zn0.1Co0.9The N intermetallic compound powder is cooled to 5K-65K under the conditions of room temperature and an external 5T magnetic field, and the generated exchange bias field ranges from 11.02kOe to 13.3 kOe.
3. Regulation Mn according to claim 13Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: when x is 0.7, adding Mn3Zn0.3Co0.7The N intermetallic compound powder is cooled to 5K-65K under the conditions of room temperature and an external 5T magnetic field, and the generated exchange bias field ranges from 1.27kOe to 6.651 kOe.
4. Regulation Mn according to claim 13Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: when x is 0.5, adding Mn3Zn0.5Co0.5The N intermetallic compound powder is cooled to 5K-65K under the conditions of room temperature and an external 5T magnetic field, and the generated exchange bias field ranges from 392Oe to 975 Oe.
5. Regulation Mn according to claim 13Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: the cooling is liquid helium cooling.
6. Regulation Mn according to claim 13Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: the Mn is3Zn1-xCoxA method for producing an N intermetallic compound, comprising the steps of:
(1)Mn2preparation of N: introducing N into Mn powder2Reacting at 730-780 ℃ to obtain Mn2N；
(2) Mn is weighed according to the molar ratio shown in the formula (1)2Grinding N powder, Zn powder and Co powder to uniformly mix all the powder; the chemical formula of the reaction is:
6Mn2N+4(1-x)Zn+4xCo→4Mn3Zn1-xCoxN+N2(formula 1)
(3) Pressing the powder into a sheet with the thickness of 2-3 mm under the pressure of 20-25 MPa;
(4) the pressed tablets were subjected to a vacuum treatment, when the vacuum reached 10-5～10-6Pa, sealing the reaction container;
(5) heating the closed reaction vessel to 750-820 ℃, preserving the heat for 80-90 hours, and then cooling to room temperature along with the furnace;
(6) mn obtained after cooling3Zn1-xCoxAn N intermetallic compound.
7. Regulation Mn of claim 63Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: in the step (1), the reaction is carried out at 730-780 ℃ and the temperature is increased to 730-780 ℃ at the rate of 10 ℃ per minute, the temperature is kept for 2700 minutes, and then the furnace is cooled to the room temperature; and the nitrogen flow is kept at 80ml/min all the time in the processes of temperature rising, heat preservation and temperature reduction.
8. Regulation Mn of claim 63Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: in the step (5), the temperature is raised to 750-820 ℃ at a rate of 10 ℃ per minute.
9. Regulation Mn of claim 63Zn1-xCoxA method of exchanging bias fields for N intermetallics, characterized by: the grinding time in the step (2) is 45-60 minutes.
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