CN115643784A - Manganese-cobalt-silicon-germanium low-temperature giant magnetostrictive material and preparation method thereof - Google Patents
Manganese-cobalt-silicon-germanium low-temperature giant magnetostrictive material and preparation method thereof Download PDFInfo
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Abstract
A low-temp. giant magnetostrictive Mn-Co-Si-Ge material is prepared from Mn, co, si and Ge, and features high toughness, high toughness and low toughness, and low cost 1‑x Ge x Wherein x is 0.06 to 0.07, the temperature of the material and the metamagnetic phase change induced by a magnetic field occur in 150K to 230K, the critical magnetic field is 0.2 to 0.8T, the low-temperature magnetostriction shows anisotropic behavior in the direction vertical to the texture and the direction parallel to the texture, the magnetostriction effect of the metamagnetic phase change induced by the 1.4T magnetic field in the direction parallel to the texture is 2026ppm at the highest, and the magnetostriction effect in the direction vertical to the texture is at the lowest1685ppm. The low-temperature magnetostrictive material prepared by the method has the advantages of low cost, low-temperature metamagnetic phase change performance, low critical magnetic field, low probability of cracking, good orientation and compact internal structure, and the application and application range of the material are expanded.
Description
Technical Field
The invention relates to the technical field of magnetic functional materials, in particular to a manganese-cobalt-silicon-germanium low-temperature giant magnetostrictive material and a preparation method thereof.
Background
With the development of science and technology, the research of low-temperature physics makes major breakthrough in the fields of superconduction, superflow, magnetic refrigeration, fractional quantum Hall effect and the like, but the research on low-temperature magnetostrictive materials is relatively less. Compared with room temperature magnetostrictive materials, the low temperature magnetostrictive material can be applied to the fields of national defense, industry and the like under low temperature conditions. At present, the most studied low-temperature magnetostrictive materials in the prior art are mainly rare earth-iron-based compounds with cubic Laves phases, and the materials have a large low-temperature magnetostrictive effect. For example, tangyanmei et al discovered PrFe 1.9 Magnetostriction of about 2500ppm can be generated at 200K under a 3T magnetic field. However, the rare earth-iron-based low-temperature magnetostrictive material has high cost due to the rare earth elements contained in the components, and the material is high in brittleness and easy to damage in the using process, so that the material is not beneficial to practical application. Therefore, it is highly desired to develop a low costThe material has low critical magnetic field and reversible low temperature giant magnetostrictive material.
MnCoSi alloys are composed of inexpensive transition group elements and main group elements and have a neel temperature (T) N ) Is about 380K. When the temperature is lower than the neel temperature, the magnetic field can induce the alloy to change magnetic phase from an antiferromagnetic phase to a ferromagnetic phase, and the larger lattice distortion is accompanied. Therefore, the material is a potential magnetostrictive material. The Mn atom determines the magnetic properties of the alloy system. And the distance between two nearest neighbors of the Mn-Mn atoms is d 1 And d 2 . The density functional theory calculation proves that d 1 The size of (a) determines the magnetic structure of the system. The positive MnCoSi alloy exhibits an antiferromagnetic structure below the Neel temperature. At 200K, the critical magnetic field for driving the metamagnetic phase change is as high as 8T, which is very unfavorable for practical application. It is very necessary to reduce the critical magnetic field. Because the antiferromagnet phase and the ferromagnetic phase in the MnCoSi alloy have a mutual dependence and mutual competition relationship, d 1 Very close to the ferromagnetic region, the anti-ferromagnetic competition relationship may be destroyed by external energy, so how to induce the anti-ferromagnetic phase in the alloy to transform to the ferromagnetic phase through certain processing steps and means, and further realize the purpose of reducing the critical magnetic field is necessary for developing the MnCoSi alloy series magnetostrictive material.
Disclosure of Invention
The technical purpose of the invention is as follows: the low-temperature magnetostrictive material which has the advantages of low cost, low-temperature metamagnetic phase change performance, low critical magnetic field, difficult cracking, good orientation and compact internal structure is prepared, so that the application and the application range are expanded.
In order to realize the purpose, the invention adopts the following technical scheme: a low-temp. giant magnetostrictive Mn-Co-Si-Ge material is prepared from Mn, co, si and Ge, and features high toughness, high toughness and low toughness, and low cost 1-x Ge x Wherein x is 0.06 to 0.07, the temperature of the material and the metamagnetic phase change induced by a magnetic field are 150 to 230K, the critical magnetic field is 0.2 to 0.8T, the low-temperature magnetostriction shows anisotropic behavior in the direction vertical to the texture direction and the direction parallel to the texture direction, and the material has the characteristic of high strength and toughness and can be used for preparing a high-strength and high-strength steel material with high strength and toughness, wherein x is 0.06 to 0.07, the temperature of the material and the metamagnetic phase change induced by the magnetic field are 150 to 230K, the critical magnetic field is 0.2 to 0.8T, the low-temperature magnetostriction shows anisotropic behavior in the direction vertical to the texture direction and the direction parallel to the texture direction, and the low-temperature magnetostriction shows anisotropic behavior in the 1.4T magnetic fieldThe maximum magnetostriction effect of the induced metamagnetic phase change in the direction parallel to the texture is 2026ppm, and the minimum magnetostriction effect in the direction vertical to the texture is-1685 ppm.
Preferably, x =0.07 in the formula.
A preparation method of a manganese-cobalt-silicon-germanium low-temperature giant magnetostrictive material comprises the following steps:
step one, according to a molecular formula of MnCoSi 1-x Ge x The molar ratio of Mn, co, si and Ge is measured, the four simple substances of Mn, co, si and Ge are respectively taken to be mixed, after being fully and evenly mixed, the mixed raw material is placed in a copper crucible in an electric arc melting furnace, and the mixture is vacuumized until the vacuum degree in the furnace is 1 multiplied by 10 -4 Pa, then repeatedly smelting the mixed raw materials for 3 to 4 times under the condition of continuously introducing high-purity argon to prepare an alloy block for later use;
step two, placing the alloy block material prepared in the step one into a quartz glass tube, then, firstly carrying out vacuum pumping treatment on the quartz glass tube, and then sealing the quartz glass tube by adopting acetylene oxygen flame;
step three, placing the quartz glass tube sealed and stored in the step two into a muffle furnace, controlling the temperature in the muffle furnace to be continuously raised from room temperature to 1227 ℃, applying a 6T strong magnetic field for strong magnetic field solidification, preserving the heat for 50-60min at the temperature, then removing the magnetic field, controlling the temperature in the muffle furnace to be reduced to 850 ℃ at the speed of 2 ℃/min, and then, taking out the prepared alloy sample for later use after the temperature in the muffle furnace is naturally reduced to room temperature;
and step four, putting the alloy sample prepared in the step three into the muffle furnace again, controlling the temperature in the muffle furnace to be continuously raised from room temperature to 850 ℃ at the heating rate of 10 ℃/min, carrying out annealing heat preservation treatment for 72-80h, then controlling the temperature in the muffle furnace to be slowly cooled to room temperature, and taking out the product to obtain the finished product of the low-temperature giant magnetostrictive material.
Preferably, in the first step, the four simple metals of Mn, co, si and Ge are weighed with a mass accuracy of 0.01mg.
Preferably, in the first step, the purity of the weighed Mn metal simple substance is more than 99%, and the purity of three metal simple substances of Co, si and Ge is more than 99.99%.
Preferably, in the step one, a circulating water cooling system is adopted to cool the electric arc melting furnace during the melting process of the electric arc melting furnace.
Preferably, in the third step, the temperature rise rate in the muffle furnace is 10 ℃/min.
The invention has the beneficial effects that:
(1) The MnCoSi prepared by the invention 1-x Ge x Compared with rare earth magnetostrictive materials, the low-temperature giant magnetostrictive material is lower in cost because of being MnCoSi metal. The material shows anisotropic behavior in the direction vertical to the texture and the direction parallel to the texture, the maximum magnetostriction in the direction parallel to the texture reaches 2026ppm, the minimum magnetostriction in the direction vertical to the texture reaches-1685 ppm, the minimum critical magnetic field can be reduced to 0.2 to 0.8T and is close to the rare earth magnetostriction material TbFe 2 . Namely: the magnetic change phase thereof is changed at low temperature, the critical magnetic field is lower, the magnetostrictive material is not easy to crack, the internal structure is compact, and the MnCoSi is promoted 1-x Ge x The application process of the alloy on the low-temperature magnetostrictive material is wide in application range.
(2) According to the preparation process, on one hand, si in the alloy is replaced by a small amount of Ge, so that the adjustment that the temperature of the metamagnetic phase change of the finished low-temperature giant magnetostrictive material is lowered is realized, and the critical magnetic field is effectively reduced. On the other hand, the method utilizes 6T high-intensity magnetic field solidification and assists the operation working step of slowly cooling at the cooling rate of 2 ℃/min, and the magnetic crystal anisotropy energy and the magnetic field strength of the particle phase in the alloy material are strong enough by heating the alloy particles to a semi-solid state with solid phase particles and a liquid matrix coexisting, and carrying out isothermal treatment for a period of time under the action of the 6T high-intensity magnetic field and then solidifying, so that the magnetic field force acting on the particle phase drives the particles to rotate and orient in the liquid matrix. After the subsequent solidification process, the orientation state of the particles is fixed to form an alloy sample with a specific orientation, and then the alloy sample is slowly cooled to prepare the compact finished product low-temperature giant magnetostrictive material with the orientation. The process has simple steps, convenient operation and excellent finished product performance.
(3) The preparation method provides a new design idea for researching the low-temperature magnetostrictive material based on the magnetic phase change mechanism.
(4) The preparation method effectively adjusts the minimum adjacent distance d of Mn-Mn atoms in the MnCoSi alloy through operations of strong magnetic field solidification, post annealing and the like after vacuum tube sealing 1 The size of the alloy is reduced, the anti-ferromagnetic phase is induced to be converted into the ferromagnetic phase, the magnetic structure of the alloy system is further changed, and the purpose of reducing the critical magnetic field of the finished product low-temperature giant magnetostrictive material is further achieved. The positive MnCoSi alloy is subjected to the large internal stress generated by martensite phase transformation in the process of furnace cooling after smelting, so that cracks appear on the surface of a sample, and the mechanical property is poor. The method comprises the steps of heating alloy raw materials to a semi-solid state in which solid-phase particles and a liquid matrix coexist, carrying out isothermal treatment for a long time under the action of a strong magnetic field, and then solidifying to enable the particle phase to complete rotational orientation and solidification positioning in the liquid matrix, so as to improve the mechanical property and the magnetostrictive property of a MnCoSi system. Then, the huge internal stress generated by martensite phase transformation is slowly released in a slow cooling mode, and MnCoSi with orientation, compact interior, difficult cracking and good mechanical property is formed 1-x Ge x Low temperature giant magnetostrictive materials.
Drawings
FIG. 1 is an XRD spectrum of the low temperature giant magnetostrictive material prepared in example 1 and example 2;
FIG. 2 is the isothermal magnetization curve of the low temperature giant magnetostrictive material prepared in example 1;
FIG. 3 is the isothermal magnetization curve of the low temperature giant magnetostrictive material prepared in example 2;
FIG. 4 is a graph showing the magnetostriction of the low temperature giant magnetostrictive material obtained in example 1;
FIG. 5 is a graph of the magnetostriction of the low temperature giant magnetostrictive material prepared in example 2.
Detailed Description
The technical solutions of the present invention will be further described with reference to the following examples so that those skilled in the art can better understand the present invention and can practice the present invention. The examples are only a part of the examples of the present invention and are not intended to limit the present invention.
A low-temp. giant magnetostrictive Mn-Co-Si-Ge material is prepared from Mn, co, si and Ge, and features high toughness, high toughness and low toughness, and low cost 1-x Ge x Wherein x is more than or equal to 0.06 and less than or equal to 0.07, the temperature of the material and the metamagnetic phase change induced by a magnetic field occur at 150K to 230K, the critical magnetic field is 0.2 to 0.8T, the low-temperature magnetostriction shows anisotropic behaviors in the direction vertical to the texture and the direction parallel to the texture, the maximum magnetostriction effect of the metamagnetic phase change under the induction of a 1.4T magnetic field in the direction parallel to the texture reaches 2026ppm, and the minimum magnetostriction effect in the direction vertical to the texture reaches-1685 ppm.
The preparation method mainly comprises the steps of smelting the prepared mixed raw materials, sealing a pipe in vacuum, solidifying by a strong magnetic field, post-annealing and the like, and specifically comprises the following steps:
taking a Mn metal simple substance with the purity of more than 99 percent, a Co metal simple substance with the purity of more than 99.99 percent, a Si metal simple substance and a Ge metal simple substance as raw materials, and preparing MnCoSi according to a molecular formula 1-x Ge x Calculating the molar ratio of Mn, co, si and Ge, calculating the mass of the required metal simple substance, mixing, weighing to 0.01mg, mixing the metal simple substances uniformly, pouring the mixed raw material into a copper crucible of an arc melting furnace, vacuumizing to the degree of vacuum of 1 × 10 in the furnace -4 Pa, then repeatedly smelting the mixed raw materials for 3 to 4 times under the condition of continuously introducing high-purity argon, and cooling the arc melting furnace by adopting a circulating water cooling system in the process to prepare an alloy block for later use;
step two, placing the alloy block material prepared in the step one into a quartz glass tube, vacuumizing by using a mechanical pump, and sealing the quartz glass tube by using acetylene oxygen flame;
step three, placing the quartz glass tube sealed and stored in the step two into a muffle furnace, controlling the temperature in the muffle furnace to be continuously increased from room temperature to 1227 ℃ at the heating rate of 10 ℃/min, applying a 6T strong magnetic field for strong magnetic field solidification, carrying out heat preservation at the temperature for 50-60min, then removing the magnetic field, controlling the temperature in the muffle furnace to be reduced to 850 ℃ at the rate of 2 ℃/min, and then, taking out the prepared alloy sample for later use after the temperature in the muffle furnace is naturally reduced to room temperature;
and step four, putting the alloy sample prepared in the step three into the muffle furnace again, controlling the temperature in the muffle furnace to be continuously raised from room temperature to 850 ℃ at the heating rate of 10 ℃/min, carrying out annealing heat preservation treatment for 72-80h, then controlling the temperature in the muffle furnace to be slowly cooled to room temperature, and taking out the alloy sample to obtain the textured finished product low-temperature giant magnetostrictive material.
Example 1:
the low-temperature giant magnetostrictive material prepared in this embodiment specifically includes the following steps:
step one, according to a molar ratio Mn: co: si: ge =1:1:0.94:0.06 mass of the required metal simple substance is calculated, the materials are mixed, the precision is 0.01mg, the metal simple substances are mixed evenly, the mixed raw materials are poured into a copper crucible of an electric arc melting furnace, and a circulating water cooling system is used for cooling the electric arc furnace. Vacuum degree of 1X 10 -4 Introducing high-purity argon under Pa, and repeatedly smelting for 3 times.
And step two, putting the smelted alloy block into a quartz glass tube, vacuumizing by using a mechanical pump, and sealing the quartz glass tube by using acetylene oxygen flame.
And step three, putting the quartz glass tube into a muffle furnace, heating the quartz glass tube to 1227 ℃ from room temperature, applying a 6T strong magnetic field, preserving the heat for 50min at the temperature, removing the magnetic field, reducing the temperature to 850 ℃ at the speed of 2 ℃/min, removing the magnetic field, and taking out an alloy sample after the furnace temperature is naturally reduced to the room temperature.
Step four, placing the sample solidified by the strong magnetic field into a muffle furnace, heating the sample to 850 ℃ from room temperature at the speed of 10 ℃/min, preserving the heat for 80 hours, then slowly cooling the sample to the room temperature, and taking out a textured finished product MnCoSi 0.94 Ge 0.06 And (3) alloy materials.
Step five, preparing a finished product MnCoSi 0.94 Ge 0.06 The alloy material is cut into a wafer with the diameter of 10mm and the thickness of 5mm along the direction vertical to the texture, and the wafer is polished and used as a sample for XRD detection.
Step six, the finished product MnCoSi is processed 0.94 Ge 0.06 The alloy material is subjected to linear cutting along the texture direction, is cut into slices with the length of 10mm, the width of 5mm and the thickness of 3mm, and is used as a sample for carrying out magnetostriction detection after polishing.
The detection results are shown in fig. 1, fig. 2 and fig. 4.
As can be seen from FIG. 1, mnCoSi after solidification orientation by a strong magnetic field is compared with that of the positively divided MnCoSi alloy powder 0.94 Ge 0.06 Partial diffraction peaks of the alloy sample are obviously inhibited, which indicates that the sample obtains a certain degree of orientation. As can be seen from FIG. 2, when the temperature is increased from 150K to 230K, under the action of the magnetic field of 0 to 1T, mnCoSi is present 0.94 Ge 0.06 The isothermal magnetization curve of the alloy sample undergoes a metamagnetic phase transition from an antiferromagnetic state to a ferromagnetic state. The minimum critical magnetic field is 0.2 to 0.8T. As can be seen from FIG. 4, under the action of a 1.4T magnetic field, mnCoSi 0.94 Ge 0.06 The magnetostrictive effect of the alloy sample shows obvious anisotropic behavior along the direction parallel to the texture and the direction vertical to the texture, the maximum magnetostrictive energy in the direction parallel to the texture reaches 2026ppm, and the minimum magnetostrictive energy in the direction vertical to the texture reaches-668 ppm.
Example 2:
the low-temperature giant magnetostrictive material prepared in the embodiment specifically comprises the following steps:
step one, according to a molar ratio Mn: co: si: ge =1:1:0.93:0.07 calculating the mass of the required metal simple substance, mixing the materials to be accurate to 0.01mg, uniformly mixing the metal simple substance, pouring the mixed raw materials into a copper crucible of an electric arc melting furnace, and cooling the electric arc furnace by a circulating water cooling system. Vacuum degree of 1X 10 -4 Introducing high-purity argon under Pa, and repeatedly smelting for 4 times.
And step two, putting the smelted alloy block into a quartz glass tube, vacuumizing by using a mechanical pump, and sealing the quartz glass tube by using acetylene oxygen flame.
And step three, putting the quartz glass tube into a muffle furnace, heating the quartz glass tube to 1227 ℃ from room temperature, applying a 6T strong magnetic field, preserving the temperature for 60min, removing the magnetic field, reducing the temperature to 850 ℃ at the speed of 2 ℃/min, removing the magnetic field, and taking out an alloy sample after the furnace temperature is naturally reduced to the room temperature.
Step four, placing the sample solidified by the strong magnetic field into a muffle furnace, heating the sample to 850 ℃ from room temperature at the speed of 10 ℃/min, preserving the heat for 72 hours, then slowly cooling the sample to the room temperature, and taking out a textured finished product MnCoSi 0.93 Ge 0.07 And (3) alloy materials.
Step five, preparing a finished product MnCoSi 0.93 Ge 0.07 The alloy material is cut into a wafer with the diameter of 10mm and the thickness of 5mm along the direction vertical to the texture, and the wafer is polished and used as a sample for XRD detection.
Step six, the finished product MnCoSi is processed 0.93 Ge 0.07 The alloy material is subjected to linear cutting along the texture direction, is cut into thin slices with the length of 10mm, the width of 5mm and the thickness of 3mm, and is used as a sample for carrying out magnetostriction detection after polishing and grinding.
The detection results are shown in fig. 1, 3 and 5.
As can be seen from FIG. 1, mnCoSi after solidification orientation by a strong magnetic field is compared with that of the positively divided MnCoSi alloy powder 0.93 Ge 0.07 Most diffraction peaks of the alloy sample are obviously suppressed, and only a (013) diffraction peak is left, which indicates that the sample obtains a higher degree of orientation. As can be seen from FIG. 3, in the process of temperature rise from 150K to 230K, under the action of 0 to 1T magnetic field, mnCoSi 0.93 Ge 0.07 The isothermal magnetization curve of the alloy sample undergoes a metamagnetic phase change from an antiferromagnet state to a ferromagnetic state, and the critical magnetic field is as low as 0.4 to 0.8T. As can be seen from FIG. 5, under the action of a 1.4T magnetic field, mnCoSi is present 0.93 Ge 0.07 The alloy sample shows obvious anisotropic behavior along the directions parallel to the texture and perpendicular to the texture, the maximum magnetostriction energy of the alloy sample in the direction parallel to the texture reaches 1933ppm, and the minimum magnetostriction energy in the direction perpendicular to the texture reaches-1685 ppm.
Claims (7)
1. A manganese cobalt silicon germanium low temperature giant magnetostrictive material is characterized in that: the material consists of four metals of Mn, co, si and Ge, and the molecular formula of the material is MnCoSi 1-x Ge x Wherein x is 0.06 to 0.07, the temperature of the material and the metamagnetic phase change induced by a magnetic field are 150 to 230K, the critical phase change field is 0.2 to 0.8T, and the low-temperature magnetostriction is vertical to the critical phase change fieldAnisotropic behavior is shown in the texture direction and the direction parallel to the texture direction, the metamagnetic phase change under the induction of a 1.4T magnetic field reaches the maximum magnetostrictive effect of 2026ppm in the direction parallel to the texture direction, and the minimum magnetostrictive effect reaches-1685 ppm in the direction vertical to the texture direction.
2. The Mn-Co-SiGe low-temperature GMT material as claimed in claim 1, wherein: x =0.07 in the formula.
3. The method of claim 1, comprising the steps of:
step one, according to a molecular formula of MnCoSi 1-x Ge x The molar ratio of Mn, co, si and Ge is measured, the four simple substances of Mn, co, si and Ge are respectively taken to be mixed, after being fully and evenly mixed, the mixed raw material is placed in a copper crucible in an electric arc melting furnace, and the mixture is vacuumized until the vacuum degree in the furnace is 1 multiplied by 10 -4 Pa, then repeatedly smelting the mixed raw materials for 3 to 4 times under the condition of continuously introducing high-purity argon to prepare an alloy block for later use;
step two, placing the alloy block material prepared in the step one into a quartz glass tube, then, firstly carrying out vacuum pumping treatment on the quartz glass tube, and then sealing the quartz glass tube by adopting acetylene oxygen flame;
step three, placing the quartz glass tube sealed and stored in the step two into a muffle furnace, controlling the temperature in the muffle furnace to be continuously raised from room temperature to 1227 ℃, applying a 6T strong magnetic field for strong magnetic field solidification, preserving the heat for 50-60min at the temperature, then removing the magnetic field, controlling the temperature in the muffle furnace to be reduced to 850 ℃ at the speed of 2 ℃/min, and then, taking out the prepared alloy sample for later use after the temperature in the muffle furnace is naturally reduced to room temperature;
and step four, putting the alloy sample prepared in the step three into the muffle furnace again, controlling the temperature in the muffle furnace to be continuously raised from room temperature to 850 ℃ at the heating rate of 10 ℃/min, carrying out annealing heat preservation treatment for 72-80h, then controlling the temperature in the muffle furnace to be slowly cooled to room temperature, and taking out the product to obtain the finished product of the low-temperature giant magnetostrictive material.
4. The method of claim 3, wherein the Mn-Co-Si-Ge low-temperature giant magnetostrictive material comprises: in the first step, the mass accuracy of the four simple metals of Mn, co, si and Ge is 0.01mg.
5. The method of claim 3, wherein the Mn-Co-Si-Ge low-temperature giant magnetostrictive material comprises: in the first step, the purity of the weighed Mn metal simple substance is more than 99%, and the purity of three metal simple substances of Co, si and Ge is more than 99.99%.
6. The method of claim 3, wherein the Mn-Co-Si-Ge low-temperature giant magnetostrictive material comprises: in the step one, a circulating water cooling system is adopted to cool the electric arc melting furnace in the process of melting by using the electric arc melting furnace.
7. The method of claim 3, wherein the Mn-Co-Si-Ge low-temperature giant magnetostrictive material comprises: in the third step, the temperature rise rate in the muffle furnace is 10 ℃/min.
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