CN110819868A - Magnetic memory alloy with long functional life and preparation method thereof - Google Patents
Magnetic memory alloy with long functional life and preparation method thereof Download PDFInfo
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Abstract
The invention provides a magnetic memory alloy with long functional life and a preparation method thereof, belonging to the field of shape memory alloys. The alloy has the chemical formula as follows: coxNiyAlzNdj(ii) a Wherein x is not less than 31.9 and not more than 39.8, y is not less than 30.1 and not more than 34.6, z is not less than 29.2 and not more than 35.7, j is not less than 0.8 and not more than 1.5, x + y + z + j is 100, and x, y, z and j represent the content in mole percentage. Compared with the prior art, the magnetic shape memory alloy of the invention is on the second part of the memory alloyCo with the formation of coherent ultra-fine particles around the two phases7Nd2The intermetallic compound strengthens the mechanical property of the second phase, greatly improves the magnetic property and the anti-functional fatigue property, ensures that the alloy has excellent mechanical property and high functional life, 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 long functional life and a preparation method thereof.
Background
Society is now rapidly developing at unprecedented rates, relying heavily on the materials, information, and energy industries in the process of development. The material plays a very important role therein. Smart materials are a new area of rapidly evolving materials technology in the world. The most widely used intelligent materials are piezoelectric materials, magnetostrictive materials and shape memory alloys. Recently, many new materials having various functions have been discovered, such as ferromagnetic ferroelectric materials, ferroelectric shape memory alloys, ferromagnetic shape memory alloys. Among them, ferromagnetic shape memory alloy has both high response frequency and large magnetic strain, and is one of ideal materials for industrial actuators.
At present, in industrial application, an executive device needs to face higher use frequency and use times, after high-frequency cyclic strain for many times, the magnetic strain function of ferromagnetic shape memory alloy which is used as a key material of an actuator gradually declines, so that the function of the actuator declines and even fails, and the industrial application and popularization of the actuator which takes the material as a core component are greatly hindered. Therefore, a novel magnetic control shape memory alloy with excellent mechanical property, larger magnetic strain and high functional fatigue life is expected to be developed to accelerate the industrial application and popularization.
Disclosure of Invention
In order to overcome the defects, the invention provides a magnetic memory alloy with long functional life and a preparation method of the magnetic memory alloy with long functional life.
In order to achieve the purpose of the invention, the technical scheme of the invention is as follows: a magnetic memory alloy having a long functional life, characterized in that: 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 long functional life, 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.5X 10-2～1×10-3A low vacuum state of MPa; b. the smelting temperature is 1550-1650 ℃; 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 represented by the formula (I) wherein the element coefficient K is 11 to 15 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 630-680 ℃; time: 7-15 hours; vacuum degree: 5X 10-2～1×10-3MPa; applying magnetic field intensity: 1X 105～5×106A·m-1(ii) a The magnetic field rise rate is: 600 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: 600 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 long functional life of the invention is characterized in that the chemical formula of the memory alloy is as follows: coxNiyAlzNdj(ii) a Wherein x is not less than 31.9 and not more than 39.8, y is not less than 30.1 and not more than 34.6, z is not less than 29.2 and not more than 35.7, j is not less than 0.8 and not more than 1.5, x + y + z + j is 100, and x, y, z and j represent the content in mole percentage.
Further, the magnetic memory alloy having a long functional life according to the present invention is characterized in that Co-ultrafine Co is formed around the second phase of the memory alloy7Nd2An intermetallic compound.
The alloy manufactured by the invention has the capability of generating deformation in a room temperature range through external magnetic field control and has longer functional life. The magnetic shape memory alloy of the invention forms coherent ultra-fine Co around the second phase7Nd2The intermetallic compound has the characteristics of good mechanical property and magnetic property, so that the alloy can have the characteristics of good mechanical property and high functional fatigue life.
Compared with the prior art, the invention has the following advantages:
the invention provides a magnetic memory alloy with long functional life, which forms coherent ultra-fine Co around the second phase of the memory alloy relative to other magnetic control shape memory alloys7Nd2The intermetallic compound strengthens the mechanical property of the second phase, greatly improves the magnetic property and the anti-functional fatigue property, ensures that the alloy has excellent mechanical property and high functional life, and greatly widens the industrial application range of the alloy.
Compared with the existing material, the magnetic memory alloy with long functional life has the advantages of excellent mechanical property and long functional life.
(1): strengthening the mechanical property: the Nd element has a high solid solubility in the Co-based alloy and is usually dissolved as interstitial atoms in the structure. However, under the process conditions of the invention patent, part of Nd element is deviated around a second phase at a grain boundary in the magnetic field heat treatment process, so that the Nd element around the second phase is supersaturated and precipitated. Meanwhile, because the second phase is a Co-rich phase, the Nd element and the Co react under the process conditions of the invention to form the coherent ultra-fine phaseCo7Nd2An intermetallic compound. The intermetallic compound has excellent comprehensive mechanical property, especially higher strength, so that the comprehensive mechanical property of the second phase of the alloy is greatly improved, and the overall mechanical property of the alloy is further enhanced.
(2): improvement of functional fatigue life: the failure to recover to the original state after the twin crystal martensite twin boundaries migrate to and fro is one of the main causes of the functional fatigue of the magnetic shape memory alloy. The invention generates more ultra-fine coherent Co around the second phase7Nd2The intermetallic compound has excellent comprehensive mechanical property, and the excellent elastoplasticity plays a role in assisting 'pushing' and 'pulling' in the process of driving the alloy twin crystal martensite to migrate and recover in an external magnetic field, so that twin crystal martensite twin boundaries can be recovered to the original state after reciprocating migration, and the functional fatigue life of the alloy is further prolonged.
(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 surface so as to enhance the processing performance of the material, such as holes and the like. Not only ensures that pure metal has enough time and temperature to melt into alloy ingot, but also ensures that Co can be formed in the subsequent water cooling process7Nd2An intermetallic compound; meanwhile, the burning loss of alloy components caused by overhigh temperature and overlong time is avoided. Lu in alloy structure2Ni17The 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, especially the second phase structure of Co and Nd aggregation, the magnetic domains are directionally arranged under the drive of the external magnetic field, thereby changing the Co and Nd aggregation7Nd2The magnetic entropy of the metal intermediate phase is improved, and Co is increased7Nd2Stability of metallic mesophases, of micron-sized Co7Nd2The metal intermediate phase can stably exist in the hairIn the second phase of the bright alloy, the preparation method not only ensures that pure metal has enough time and temperature to be melted into an alloy ingot, but also ensures that stable Co can be formed in the subsequent water cooling process7Nd2An intermetallic compound. Meanwhile, the burning loss of alloy components caused by overhigh temperature and overlong time can be avoided.
(4): the heat treatment method comprises the following steps: the heat treatment adopts vacuum magnetic field heat treatment, on one hand, the reduction of mechanical property and magnetic property of the alloy caused by surface oxidation in the high-temperature heat treatment process can be effectively avoided, for example: the magnetic strain of the oxidized alloy can be greatly reduced and the martensitic transformation temperature can be changed. On the other hand, the magnetic domain pair in the alloy can be orderly in direction by applying magnetic field heat treatment, so that induced anisotropy is caused, the magnetocrystalline anisotropy of the alloy is improved, and the phenomenon of magnetic domain dispersion caused by overlarge magnetic field intensity and magnetic field rising rate is avoided. And then cooling along with the furnace and slowly removing the magnetic field, so that on one hand, the internal stress of the alloy can be reduced through slow cooling, and on the other hand, the direction preference of a magnetic domain in the alloy can be kept all the time in the cooling process.
In summary, the present invention provides a magnetic memory alloy with a long functional life and a method for preparing the same, and the alloy has the advantages of excellent mechanical properties and a long functional life compared with the existing materials.
Drawings
FIG. 1 shows Co of the present inventionxNiyAlzNdjSEM 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 Co35.6Ni33.2Al30.4Nd0.8The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Nd with the purity of 99.99 percent;
s2, smelting: placing the prepared raw materials in a crucibleThe vacuum melting is carried out, and the melting conditions are as follows: a.5X 10-2A low vacuum state of MPa; b. the smelting temperature is 1550 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 330s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 11s 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 630 ℃; time: 15 hours; vacuum degree: 5X 10-2MPa; applying magnetic field intensity: 1X 105A·m-1(ii) a The magnetic field rise rate is: 600 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: 600 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 Co39.8Ni30.1Al29.2Nd0.9The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Nd 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.6X 10-2A low vacuum state of MPa; b. the smelting temperature is 1570 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 339s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 12s 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 640 ℃; time: 14 hours; vacuum degree: 6X 10-2MPa; applying magnetic field intensity: 5X 105A·m-1(ii) a The magnetic field rise rate is: 600 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.1 ℃ s-1(ii) a The magnetic field reduction rate was: 600 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 Co31.9Ni31.3Al35.7Nd1.1The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Nd 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.7X 10-2A low vacuum state of MPa; b. the smelting temperature is 1580 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 344s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 13s 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 650 ℃; time: 13 hours; vacuum degree: 7X 10-2MPa; applying magnetic field intensity: 1X 106A·m-1(ii) a The magnetic field rise rate is: 600 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.2 ℃ s-1(ii) a The magnetic field reduction rate was: 600 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 Co32.7Ni34.6Al31.5Nd1.2The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Nd 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.8X 10-2A low vacuum state of MPa; b. the smelting temperature is 1590 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 343s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 14s 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 660 ℃; time: 12 hours; vacuum degree: 8X 10-2MPa; applying magnetic field intensity: 2X 106A·m-1(ii) a The magnetic field rise rate is: 600 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.3 ℃ s-1(ii) a The magnetic field reduction rate was: 600 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 Co37.5Ni30.9Al30.7Nd1.4The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Nd 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.9X 10-2A low vacuum state of MPa; b. the smelting temperature is 1600 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 324s (according to the formula t ═ Kx (M)-1/2) To obtain a compound of formula (I), wherein the element coefficient K is 14.5 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 670 ℃; time: 10 hours; vacuum degree: 9X 10-2MPa; applying magnetic field intensity:4×106A·m-1(ii) a The magnetic field rise rate is: 600 A.m-1·s-1；
S4, cooling; and then cooling along with the furnace, wherein the cooling speed range is as follows: 0.4 ℃ s-1(ii) a The magnetic field reduction rate was: 600 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.
Example 6:
preparation of 400g of a composition Co32.3Ni32.8Al33.4Nd1.5The preparation method of the low-fatigue magnetic memory alloy comprises the following steps:
s1, material preparation: respectively weighing Co, Ni, Al and Nd 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 10-3A low vacuum state of MPa; b. the smelting temperature is 1650 ℃; c. magnetic stirring is adopted in the smelting process; d. the melting time was 300s (according to the formula t ═ Kx (M)-1/2) To obtain a coefficient of element K of 15s 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 680 ℃; time: 7 hours; vacuum degree: 1X 10-3MPa; applying magnetic field intensity: 5X 106A·m-1(ii) a The magnetic field rise rate is: 600 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: 600 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. The results of the tests of examples 1 to 6 are shown in Table 1.
TABLE 1 Co of different compositionsxNiyAlzNdjMechanics of materialsPerformance and functional fatigue life
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 long functional life, characterized in that: the raw materials and the mixture ratio are as follows by mol percent:
the preparation process of the magnetic memory alloy with the long functional life 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.5X 10-2～1×10- 3A low vacuum state of MPa; b. the smelting temperature is 1550-1650 ℃; 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 represented by the formula (I) wherein the element coefficient K is 11 to 15 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 630-680 ℃; time: 7-15 hours; vacuum degree: 5X 10-2～1×10-3MPa; applying a magnetic field strength; 1X 105～5×106A·m-1(ii) a The magnetic field rise rate is: 600 A.m-1·s-1；
S4, cooling; then cooling with the furnaceThe cooling speed range is as follows: 0.01 to 0.5 ℃ s-1(ii) a The magnetic field reduction rate was: 600 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 long functional life, characterized in that the memory alloy has the chemical formula: coxNiyAlzNdj(ii) a Wherein x is not less than 31.9 and not more than 39.8, y is not less than 30.1 and not more than 34.6, z is not less than 29.2 and not more than 35.7, j is not less than 0.8 and not more than 1.5, x + y + z + j is 100, and x, y, z and j represent the content in mole percentage.
3. A magnetic memory alloy having a long functional life, characterized in that a coherent ultra-fine Co is formed around a second phase of the memory alloy7Nd2An intermetallic compound.
4. A magnetic memory alloy having a high functional lifetime as claimed in claim 2, wherein said memory alloy is obtained by the method of claim 1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002129273A (en) * | 2000-08-14 | 2002-05-09 | Kiyohito Ishida | Ferromagnetic shape memory alloy and actuator using the same |
| EP1460139A1 (en) * | 2003-03-18 | 2004-09-22 | HONDA MOTOR CO., Ltd. | Co-Ni-Al Shape memory alloy and method for producing same |
| 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 |
| CN107586979A (en) * | 2017-09-28 | 2018-01-16 | 南京工程学院 | A kind of microalloying of rare earth high conductivity copper alloy and preparation method thereof |
-
2018
- 2018-08-10 CN CN201810931826.8A patent/CN110819868A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002129273A (en) * | 2000-08-14 | 2002-05-09 | Kiyohito Ishida | Ferromagnetic shape memory alloy and actuator using the same |
| EP1460139A1 (en) * | 2003-03-18 | 2004-09-22 | HONDA MOTOR CO., Ltd. | Co-Ni-Al Shape memory alloy and method for producing same |
| 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 |
| CN107586979A (en) * | 2017-09-28 | 2018-01-16 | 南京工程学院 | A kind of microalloying of rare earth high conductivity copper alloy and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JIA JU, ET AL.: "Microtructure and Magnetic Property Variation with Addition of Rare Earth Element Dy in Co-Ni-Al Ferromagnetic Shape Memory Alloy", 《JOURNAL OF IRON AND STEEL RESEARCH, INTERNATIONAL》 * |
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