CN110819871A - Magnetic memory alloy with low starting threshold value and preparation method thereof - Google Patents
Magnetic memory alloy with low starting threshold value and preparation method thereof Download PDFInfo
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Abstract
The invention provides a magnetic memory alloy with low starting threshold value and a preparation method thereof, and compared with the existing material, the alloy has the advantages of excellent mechanical property and low starting threshold value of magnetic strain. The alloy has the chemical formula as follows: coxAlyNizPrj(ii) a Wherein x is more than or equal to 32.8 and less than or equal to 39.7, y is more than or equal to 32.5 and less than or equal to 37.6, z is more than or equal to 28.3 and less than or equal to 32.4, j is more than or equal to 0.6 and less than or equal to 1.2, x + y + z + j is 100, and x, y, z and j represent the content in mole percentage. Compared with the prior material, the magnetic control shape memory alloy of the invention forms coherent ultra-fine dispersion distribution Co in the matrix phase of the alloy19Pr5The intermetallic compound ensures that the alloy has the characteristics of good mechanical property and magnetic property, promotes the alloy to have the characteristics of good mechanical property and low starting threshold value, and greatly widens the industrial application range of the alloy.
Description
Technical Field
The invention belongs to the field of shape memory alloys, and particularly relates to a magnetic memory alloy with a low starting threshold value and a preparation method thereof.
Background
Ferromagnetic shape memory alloys are a new class of shape memory alloys that developed in the last 90 th century. The novel alloy has thermoelastic martensite phase transformation and ferromagnetic transformation, the shape memory effect can be performed under the control of a magnetic field, and the magnetic strain cannot be influenced by the thermal conductivity and the heat dissipation condition of the alloy. Compared with the traditional temperature control shape memory alloy, the ferromagnetic shape memory alloy has the advantages of large strain and high response frequency. Therefore, the ferromagnetic shape memory alloy has great potential to become the first choice of the next generation of intelligent materials and is widely applied to high and new technical fields such as mechanical engineering, spin electronics, intelligent sensors and the like.
At present, the experimental and theoretical research on ferromagnetic shape memory alloys at home and abroad is continuously developed, and in the magnetic shape memory alloy, the formation of twin boundaries is generated by the non-diffusion type martensite phase transformation from high-symmetry austenite at high temperature to low-temperature low-symmetry martensite. Because the martensite phase of the alloy has strong magnetic anisotropy, the magnetic moment of the martensite phase is arranged along the direction of the easy magnetization axis, and the direction of the magnetization intensity is changed when the martensite phase crosses the twin boundary. In the absence of a magnetic field, the direction of magnetization in the martensitic modification is aligned along the easy axis direction to lower the static magnetic energy. After the external magnetic field is applied, the magnetization direction of the martensite modification will tend to the direction of the external magnetic field to reduce the zeeman energy. If the magnetic anisotropy is weak, the magnetization will be turned to the direction of the external magnetic field, resulting in magnetostriction. However, because the magnetic strain starting threshold of the existing ferromagnetic shape memory alloy under an external magnetic field is high, a sensor or an electronic device prepared from the alloy can generate obvious magnetic strain only under the intervention of a strong magnetic field, and the use conditions and requirements of the electronic device are increased seriously, so that the development of a novel magnetic control shape memory alloy with good mechanical property, large magnetic strain and low strain starting threshold is expected to accelerate the industrial application and popularization of the novel magnetic control shape memory alloy.
Disclosure of Invention
In order to overcome the defects, the invention provides a magnetic memory alloy with a low starting threshold value and a preparation method of the magnetic memory alloy with the low starting threshold value.
In order to achieve the purpose of the invention, the technical scheme of the invention is as follows: a magnetic memory alloy having a low activation threshold, comprising: the raw materials and the mixture ratio are as follows by mol percent:
the invention also discloses a preparation process of the magnetic memory alloy with the low starting threshold, which is characterized by comprising the following specific steps of:
s1, material preparation: proportioning and weighing according to the proportion;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.1X 10-3～5×10-3A low vacuum state of MPa; b. the smelting temperature is 1600-1700 ℃; c. magnetic stirring is adopted in the smelting process; d. melting time is according to the formula t ═ K × (M)-1/2) Obtained by the reaction of a compound of formula (I) wherein the element coefficient K is 5 to 9 s.g-1/2M isThe mass of the smelted alloy is g; t is melting time in units of s;
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 660-750 ℃; time: 10-15 hours; vacuum degree: 1X 10-3～5×10-3MPa; applying magnetic field intensity: 1X 106～6×107A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.01 to 0.5 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
Further, the magnetic memory alloy with low starting threshold value is characterized in that the chemical formula of the memory alloy is as follows: coxAlyNizEuj(ii) a Wherein x is more than or equal to 32.8 and less than or equal to 39.7, y is more than or equal to 32.5 and less than or equal to 37.6, z is more than or equal to 28.3 and less than or equal to 32.4, j is more than or equal to 0.6 and less than or equal to 1.2, x + y + z + j is 100, and x, y, z and j represent the content in mole percentage.
Further, the magnetic memory alloy with low starting threshold is characterized in that coherent ultra-fine dispersion distribution Co is formed in the matrix phase of the memory alloy19Pr5An intermetallic compound.
The alloy manufactured by the invention has the capability of generating deformation by low external magnetic field driving in a room temperature range, and is a magnetic memory alloy with low starting threshold. Co with coherent ultra-fine dispersion distribution is formed in the matrix phase of the magnetic memory alloy19Pr5The intermetallic compound ensures that the alloy has the characteristics of good mechanical property and magnetic property, and promotes the alloy to have the characteristics of good mechanical property and low starting threshold value.
Compared with the prior art, the invention has the following advantages:
the invention provides a magnetic memory alloy with low starting threshold, which forms coherent ultra-fine dispersion distribution in a matrix phase of the alloy relative to other magnetic control shape memory alloysCo19Pr5The intermetallic compound ensures that the alloy has the characteristics of good mechanical property and magnetic property, promotes the alloy to have the characteristics of good mechanical property and low starting threshold value, and greatly widens the industrial application range of the alloy.
Compared with the existing material, the magnetic memory alloy with low starting threshold has the advantages of excellent mechanical property and low starting threshold of magnetic strain.
(1): excellent mechanical properties: pr has a larger atomic radius and special physical and chemical properties, and basically has lower solid solubility in a matrix phase in the Co-Ni-Al ternary alloy, and the added Pr is separated out in the matrix phase to form a brittle precipitate with deteriorated mechanical properties. However, under the process conditions of the invention patent, Pr atoms precipitated from the matrix phase are not precipitated in the form of brittle phase any more, but react with Co element to form Co with good mechanical property19Pr5The intermetallic compound greatly improves the mechanical property of the alloy. .
(2): the magnetic strain becomes low activation threshold: the magnetic shape and the magnetic strain starting threshold of the alloy are greatly influenced by magnetic parameters such as magnetocrystalline anisotropy, saturation magnetization and the like of the alloy. Co formed in the patent of the invention19Pr5The intermetallic compound has excellent magnetic properties, and particularly has saturation magnetization 5-6 times that of the alloy. Precipitating a large amount of Co in the alloy matrix phase19Pr5The intermetallic compound greatly improves the saturation magnetization of the alloy, so that the alloy can obtain larger strain driving force in a lower magnetic field. Thus, the coherent ultra-fine dispersion of Co present in the matrix phase of the present invention19Pr5The intermetallic compound can greatly reduce the magnetic strain of the alloy and lower the starting threshold.
(3): the preparation method comprises the following steps: the invention adopts the vacuum crucible for smelting, and in the smelting process, because the system is in a vacuum state, the mechanical and magnetic properties of the alloy are prevented from being reduced due to surface oxidation. Compared with the traditional method, the method also has the effect of gathering the internal smelting defects of the alloy to the surfaceThe processing performance of the material is enhanced, such as holes and the like. The perfect matching of the melting temperature and the melting time not only ensures that pure metal has enough time and temperature to be melted into alloy ingots, but also can avoid the burning loss of alloy components caused by overhigh temperature and overlong time. Co in alloy structure19Pr5The metallic mesophase belongs to an unstable metallic mesophase, which has a tendency to decompose at the solidification stage and cannot be retained in the alloy structure by conventional means. However, the invention adopts a magnetic field vacuum heat treatment mode, and induces the magnetic domains in the alloy to present obvious preferential distribution in an external magnetic field mode, particularly the Co and Pr gathered matrix phase structure, and the magnetic domains are directionally arranged under the drive of the external magnetic field, thereby changing the Co and Pr gathering matrix phase structure19Pr5The magnetic entropy of the metal intermediate phase is improved by Lu2Ni17Stability of metallic mesophase, Co-dispersed ultrafine19Pr5The metallic mesophase is capable of being stably present in the matrix phase of the alloy of the invention. In addition, the magnetic domain after orientation distribution further strengthens the magnetocrystalline anisotropy of the alloy.
In conclusion, the invention provides the magnetic memory alloy with the low starting threshold value and the preparation method thereof, and the alloy has the advantages of excellent mechanical property and low starting threshold value of magnetic strain compared with other magnetic control shape memory alloys.
Drawings
FIG. 1 shows Co of the present inventionxNiyAlzPrjSEM images of the alloys at room temperature;
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
preparation of 900g of a composition Co34.9Ni34.8Al29.7Pr0.6The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Pr with the purity of 99.99 percent;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.1X 10-3Low in MPaA vacuum state; b. the smelting temperature is 1600 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 150s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 5s g-1/2M is 900 g);
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 660 ℃; time: 15 hours; vacuum degree: 1X 10-3MPa; applying magnetic field intensity: 1X 106A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.01 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
The polycrystalline sample prepared by the above method was cut into a 5X 8mm sample by wire cutting to examine various characteristic curves.
Example 2:
preparation of 800g of a composition Co33.1Ni35.3Al30.9Pr0.7The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Pr with the purity of 99.99 percent;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.2X 10-3A low vacuum state of MPa; b. the smelting temperature is 1620 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 170s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 6s g-1/2M is 800 g);
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 670 ℃; time: 14 hours; vacuum degree: 2X 10-3MPa; applying magnetic field intensity: 5X 106A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.12 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
The polycrystalline sample prepared by the above method was cut into a 5X 8mm sample by wire cutting to examine various characteristic curves.
Example 3:
preparation of 700g of composition Co33.4Ni33.4Al32.4Pr0.8The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Pr with the purity of 99.99 percent;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.3X 10-3A low vacuum state of MPa; b. the smelting temperature is 1640 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 185s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 7s g-1/2M is 700 g);
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 680 ℃; time: 13 hours; vacuum degree: 3X 10-3MPa; applying magnetic field intensity: 1X 107A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.22 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
The polycrystalline sample prepared by the above method was cut into a 5X 8mm sample by wire cutting to examine various characteristic curves.
Example 4:
preparation of 600g of a composition of Co32.8Ni37.6Al28.7Pr0.9The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Pr with the purity of 99.99 percent;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.4X 10-3A low vacuum state of MPa; b. the smelting temperature is 1660 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 196s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 8s g-1/2M is 600 g);
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 690 ℃; time: 12 hours; vacuum degree: 4X 10-3MPa; applying magnetic field intensity: 2X 107A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.33 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
The polycrystalline sample prepared by the above method was cut into a 5X 8mm sample by wire cutting to examine various characteristic curves.
Example 5:
preparation of 500g of composition Co39.7Ni31.0Al28.3Pr1.0The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Pr with the purity of 99.99 percent;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.4.5X 10-3A low vacuum state of MPa; b. the smelting temperature is 1680 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 190s (according to the formula t ═ Kx (M)-1/2) To obtain a compound of formula (I), wherein the element coefficient K is 8.5 s.g-1/2M is 500 g);
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 700 ℃; time: 11 hours; vacuum degree: 4.5X 10-3MPa; applying magnetic field intensity: 4X 107A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.42 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
The polycrystalline sample prepared by the above method was cut into a 5X 8mm sample by wire cutting to examine various characteristic curves.
Example 6:
preparation of 400g of a composition Co35.8Ni32.5Al30.5Pr1.2The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Pr with the purity of 99.99 percent;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.5X 10-3A low vacuum state of MPa; b. the smelting temperature is 1700 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 180s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 9s g-1/2M is 400 g);
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 750 ℃; time: 10 hours; vacuum degree: 5X 10-3MPa; applying magnetic field intensity: 6X 107A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.5 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
The polycrystalline sample prepared by the above method was cut into a sample of 5X gmm by wire cutting to examine various characteristic curves.
The results of the tests of examples 1 to 6 are shown in Table 1.
TABLE 1 Co of different compositionsxNiyAlzPrjMechanical properties and magnetostriction of materialsStarting magnetic field intensity
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention.
Claims (4)
1. A magnetic memory alloy having a low activation threshold, comprising: the raw materials and the mixture ratio are as follows by mol percent:
the preparation process of the magnetic memory alloy with the low starting threshold is characterized by comprising the following specific steps of:
s1, material preparation: proportioning and weighing according to the proportion;
s2, smelting: putting the prepared raw materials into a crucible for vacuum melting, wherein the melting conditions are as follows: a.1X 10-3～5×10- 3A low vacuum state of MPa; b. the smelting temperature is 1600-1700 ℃; c. magnetic stirring is adopted in the smelting process; d. melting time is according to the formula t ═ K × (M)-1/2) Obtained by the reaction of a compound of formula (I) wherein the element coefficient K is 5 to 9 s.g-1/2M is the mass of the alloy being smelted and is given in g; t is melting time in units of s;
s3, magnetic field heat treatment: carrying out vacuum magnetic field heat treatment on the alloy ingot obtained by vacuum melting under the following treatment conditions: the temperature is 660-750 ℃; time: 10-15 hours; vacuum degree: 1X 10-3～5×10-3MPa; applying magnetic field intensity: 1X 106～6×107A·m-1(ii) a The magnetic field rise rate is: 800 A.m-1·s-1；
S4, cooling; subsequent furnace cooling, cooling rate rangeComprises the following steps: 0.01 to 0.5 ℃ s-1(ii) a The magnetic field reduction rate was: 800 A.m-1·s-1(ii) a And cooling to room temperature and taking out to obtain the final magnetic memory alloy.
2. A magnetic memory alloy with a low starting threshold is characterized in that the chemical formula of the memory alloy is as follows: coxAlyNizEuj(ii) a Wherein x is more than or equal to 32.8 and less than or equal to 39.7, y is more than or equal to 32.5 and less than or equal to 37.6, z is more than or equal to 28.3 and less than or equal to 32.4, j is more than or equal to 0.6 and less than or equal to 1.2, x + y + z + j is 100, and x, y, z and j represent the content in mole percentage.
3. A magnetic memory alloy with low starting threshold value is characterized in that Co with coherent ultra-fine dispersion distribution is formed in a matrix phase of the memory alloy19Pr5An intermetallic compound.
4. A magnetic memory alloy with a low activation threshold as claimed in claim 2, wherein the memory alloy is prepared by the method of claim 1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008030517A1 (en) * | 2006-09-06 | 2008-03-13 | Cook Incorporated | Nickel-titanium alloy including a rare earth element |
| CN103952615A (en) * | 2014-04-30 | 2014-07-30 | 东南大学 | Magnetic material with magnetic field for driving martensite twin crystal rearrangement and preparation method thereof |
| CN105755345A (en) * | 2016-04-05 | 2016-07-13 | 南京工程学院 | Rare earth magnetic material with magnetic field controlled deformation and preparation method thereof |
| CN105803266A (en) * | 2016-04-05 | 2016-07-27 | 南京工程学院 | Rare earth magnetic-control shape memory alloy low in starting critical stress and preparation method thereof |
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2018
- 2018-08-10 CN CN201810931829.1A patent/CN110819871A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008030517A1 (en) * | 2006-09-06 | 2008-03-13 | Cook Incorporated | Nickel-titanium alloy including a rare earth element |
| CN103952615A (en) * | 2014-04-30 | 2014-07-30 | 东南大学 | Magnetic material with magnetic field for driving martensite twin crystal rearrangement and preparation method thereof |
| CN105755345A (en) * | 2016-04-05 | 2016-07-13 | 南京工程学院 | Rare earth magnetic material with magnetic field controlled deformation and preparation method thereof |
| CN105803266A (en) * | 2016-04-05 | 2016-07-27 | 南京工程学院 | Rare earth magnetic-control shape memory alloy low in starting critical stress and preparation method thereof |
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