CN111057959A - Magnetostrictive material and preparation process thereof - Google Patents
Magnetostrictive material and preparation process thereof Download PDFInfo
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- CN111057959A CN111057959A CN201911233060.7A CN201911233060A CN111057959A CN 111057959 A CN111057959 A CN 111057959A CN 201911233060 A CN201911233060 A CN 201911233060A CN 111057959 A CN111057959 A CN 111057959A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10N35/00—Magnetostrictive devices
- H10N35/80—Constructional details
- H10N35/85—Magnetostrictive active materials
Abstract
The invention belongs to the field of metal magnetic materials, and particularly relates to a magnetostrictive material and a preparation process thereof, wherein the magnetostrictive material comprises the following components: nd (Fe)1‑xCox)2(ii) a Wherein x is 0.1 to 0.4. The invention uses partial Co to replace partial Fe to stabilize cubic Laves phase compound for easier synthesis, and on the other hand, partial Co to replace partial Fe can change the anisotropy of the compound to improve RFe2Magnetostrictive properties of the compound.
Description
Technical Field
The invention relates to a magnetostrictive material and a preparation process thereof, belonging to the field of metal magnetic materials.
Background
The rare earth magnetic functional material has the function of converting electromagnetic energy into mechanical energy, is widely applied to high-tip precision instruments such as sonar sensors, actuators, sensors, radars, artificial intelligence and the like, and is greatly determined to be applied in the civil field, the national defense field and the like. Rare earth magnetostrictive material, mainly RFe2(R is rare earth) Fe-based C15Laves phase rare earth intermetallic compound. The Fe-based C15Laves phase rare earth intermetallic compound is represented by Terfenol-D, and the composition component of the Fe-based C15Laves phase rare earth intermetallic compound is Tb0.27Dy0.73Fe2. The inventors of this material are U.S. a.e. clark et al and h.t. savage et al, which have separately filed U.S. patents with patent numbers 3949351, respectivelyAnd 4308474. Toshiba Japan, in addition to Terfenol-D material, a giant magnetostrictive material containing a small amount of Mn is obtained by adding a small amount of Mn instead of Fe, and this material is also patented as Showa 55-134150.
However, the rare earth metals R in the raw material components of the materials are all high-purity rare earth metals Tb, Dy, Ho and the like, the purity of the materials is more than 99.9 percent, and the smelting of master alloys and the manufacturing of oriented polycrystalline samples need high-cost equipment, so that the price of the commercialized magnetostrictive materials such as Terfenol-D is very high. There is therefore a need to find relatively inexpensive and abundant rare earth materials to replace. Single ion model calculation shows that NdFe2The magnetostriction coefficient at absolute zero can reach 2000 ppm. In addition, the light rare earth Nd has rich resources and low price. But due to Nd3+Large ionic radius, and synthesizing NdFe under normal pressure or high temperature2Alloy Laves single phases were almost unsuccessful.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a magnetostrictive material and a preparation process thereof.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a magnetostrictive material comprising the following composition: nd (Fe)1-xCox)2And x is 0.1-0.4 calculated according to the atomic ratio.
Further, amorphous or amorphous and nanocrystalline mixture bands are obtained by a melt rapid quenching method, and the cubic Laves single-phase compound is obtained by low-temperature annealing.
The invention also provides a preparation process of the magnetostrictive material, which comprises the following steps:
preparing raw materials: rare earth Nd and transition metals Fe and Co are adopted according to the stoichiometric formula Nd (Fe)1-xCox)2Proportioning by atomic ratio; wherein x is 0.1-0.4;
conventional vacuum arc melting: putting the metal simple substance obtained in the step into a copper crucible in a vacuum arc melting furnace cavity, closing the furnace cavity, pre-pumping by using a mechanical pump and continuously pumping by using a molecular pump until the vacuum degree in the furnace cavity reaches below 10-5Pa, and filling argon protective gas to the pressure of 0.06-0.09MPa lower than the atmospheric pressure; repeating the conventional smelting for 4 times until the alloy components are uniform;
quick cooling and smelting: changing the circulating water to an ice water mode, carrying out electric arc melting on the alloy to a molten state, carrying out high-speed electromagnetic stirring on the molten alloy material, maintaining for 10-20 seconds, quickly closing electric arc current, maintaining high-speed electromagnetic stirring for 5-10 seconds, and cooling the material to room temperature;
carrying out rapid quenching in a high-frequency heating single-roller rapid quenching furnace under the protection of argon;
and (3) vacuum annealing: and taking out the material and carrying out vacuum annealing to obtain the cubic Laves single-phase compound.
Further, the vacuum annealing temperature is 500-600 ℃.
Furthermore, the purity of Nd, Fe and Co is more than 99.9%.
Furthermore, the conventional vacuum arc melting adopts a mode of placing rare earth on a lower transition metal and a mode of placing transition metal on an upper transition metal.
Further, in the rapid quenching step, the linear velocity of the surface of the wheel is within the range of 20-45 m/s.
Further, the time of the vacuum annealing is 30 minutes or more.
Has the advantages that:
the invention uses partial Co to replace partial Fe to stabilize cubic Laves phase compound for easier synthesis, and on the other hand, partial Co to replace partial Fe can change the anisotropy of the compound to improve RFe2Magnetostrictive properties of the compound.
The invention utilizes the method of melt rapid quenching and subsequent annealing to synthesize Nd (Fe, Co) with high Nd content which is difficult to synthesize by the conventional method2Cubic Laves single phase.
Drawings
FIG. 1 shows Nd (Fe)0.7Co0.3)2An X-ray map of the alloy; (a) nd (Fe)0.7Co0.3)2Alloy ingot, (b)40m/s rapid quenching, (c)40m/s rapid quenching, and annealing at 500 ℃ for 30 minutes;
FIG. 2 shows Nd (Fe)0.7Co0.3)2Saturation magnetization intensity of the alloy after rapid quenching and annealing;
FIG. 3 shows Nd (Fe)0.7Co0.3)2After alloy rapid quenching annealing (lambda)||-λ⊥) In relation to the magnetic field.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
A magnetostrictive material, comprising the following components: nd (Fe)1-xCox)2Wherein x is 0.1 to 0.4. Obtaining amorphous or amorphous and nanocrystalline mixture strips by a melt rapid quenching method, and then annealing at low temperature for more than 30 minutes to obtain the cubic Laves single-phase compound.
The preparation process of the magnetostrictive material comprises the following steps:
preparing raw materials: rare earth Nd with the purity of 99.9 percent and transition metals Fe and Co with the purity of 99.9 percent are adopted according to the stoichiometric formula Nd (Fe)1-xCox)2Proportioning by atomic ratio; wherein x is 0.1-0.4;
conventional vacuum arc melting: placing the metal simple substance obtained in the step into a copper crucible in a vacuum arc melting furnace cavity, and adopting a placement mode of rare earth on the lower part and transition metal on the upper part; closing the furnace chamber, pre-pumping by using a mechanical pump and continuously pumping by using a molecular pump until the vacuum degree in the furnace chamber reaches below 10-5Pa, and introducing argon protective gas until the pressure is 0.06-0.09MPa lower than the atmospheric pressure; repeating the conventional smelting for 4 times until the alloy components are uniform;
quick cooling and smelting: the circulating water is switched to an ice water mode, namely, ice water with the temperature of 0 ℃ is adopted as the circulating water; arc melting the alloy to a molten state, electromagnetically stirring the molten alloy material at a high speed for 10-20 seconds, rapidly closing the arc current, electromagnetically stirring at a high speed for 5-10 seconds, and cooling the material to room temperature;
and (3) carrying out rapid quenching in a high-frequency heating single-roller rapid quenching furnace under the protection of argon, wherein the surface linear velocity of the wheel is adjustable within the range of 20-45 m/s.
And (3) vacuum annealing: and taking out the material and carrying out vacuum annealing at 500-600 ℃ to obtain the cubic Laves single-phase compound.
Example 2
Component Nd (Fe)0.8Co0.2)2The rapid quenching annealed alloy of (1). The prepared raw materials are put into a copper crucible for electric arc melting, the copper crucible is firstly cooled by conventional water circulation, and the alloy base metal with uniform components is obtained by repeatedly melting for 4 times in a mode of electric arc melting and electromagnetic stirring. The circulating water is switched to an ice water mode, namely, ice water with the temperature of 0 ℃ is adopted as the circulating water; the alloy is melted by electric arc melting, the melted alloy material is stirred by high-speed electromagnetism, the electric arc current is closed rapidly after being maintained for 10 seconds, and the high-speed electromagnetism stirring is maintained for 5 seconds, so that the alloy is cooled rapidly. The alloy is rapidly quenched in a high-frequency heating single-roller rapid quenching furnace under the protection of argon, and the linear velocity of the surface of the wheel is 40 m/s. And then taking out the material obtained by quick quenching and carrying out vacuum annealing at 500 ℃ to obtain the cubic Laves single-phase compound. FIG. 2 shows Nd (Fe)0.7Co0.3)2The saturation magnetization of the alloy after the rapid quenching annealing is 66emu/g, and the insert of FIG. 3 shows Nd (Fe)0.7Co0.3)2The magnetic shrinkage of the alloy after rapid quenching and annealing is 180 ppm.
Example 3
Component Nd (Fe)0.7Co0.3)2The rapid quenching annealed alloy of (1). The prepared raw materials are put into a copper crucible for electric arc melting, the copper crucible is firstly cooled by conventional water circulation, and the alloy base metal with uniform components is obtained by repeatedly melting for 4 times in a mode of electric arc melting and electromagnetic stirring. The circulating water is switched to an ice water mode, namely, ice water with the temperature of 0 ℃ is adopted as the circulating water; the alloy is melted by electric arc melting, the melted alloy material is stirred by high-speed electromagnetism, the electric arc current is closed rapidly after being maintained for 10 seconds, and the high-speed electromagnetism stirring is maintained for 5 seconds, so that the alloy is cooled rapidly. The alloy is rapidly quenched in a high-frequency heating single-roller rapid quenching furnace under the protection of argon, and the linear velocity of the surface of the wheel is 40 m/s. Then taking out the material obtained by quick quenching and carrying out vacuum annealing at 500 ℃ to obtainTo cubic Laves single phase compounds. FIG. 1 shows Nd (Fe)0.7Co0.3)2An X-ray map of the alloy; wherein (a) is Nd (Fe)0.7Co0.3)2XRD patterns of alloy ingots, (b) is XRD pattern of material obtained by 40m/s rapid quenching, and as can be seen from FIGS. 1(a) and (b), single-phase Nd (Fe) can not be obtained by direct smelting or simple rapid quenching after smelting0.7Co0.3)2An alloy compound; FIG. 1(c) is an XRD pattern of annealing at 500 ℃ for 30 minutes after 40m/s rapid quenching, and it can be seen from this figure that the method of melting rapid quenching annealing can obtain single-phase Nd (Fe)0.7Co0.3)2An alloy compound. FIG. 2 shows Nd (Fe)0.7Co0.3)2The saturation magnetization of the rapidly quenched and annealed alloy of (1) shows that Nd (Fe)0.7Co0.3)2The magnetization of the alloy compound tended to saturate when the applied magnetic field strength increased to around 14kOe, and the saturation magnetization was 60 emu/g. FIG. 3 shows Nd (Fe)0.7Co0.3)2The graph of the relationship of the magnetostriction flux-out field H of the rapidly quenched and annealed alloy. As seen from the figure, Nd (Fe)0.7Co0.3)2The magnetostriction lambda a of the alloy compound is close to saturation when the applied magnetic field strength is about 14kOe, and the magnetostriction value can reach 250 ppm.
Example 4
Component Nd (Fe)0.6Co0.4)2The rapid quenching annealed alloy of (1). The prepared raw materials are put into a copper crucible for electric arc melting, the copper crucible is firstly cooled by conventional water circulation, and the alloy base metal with uniform components is obtained by repeatedly melting for 4 times in a mode of electric arc melting and electromagnetic stirring. The circulating water is switched to an ice water mode, namely, ice water with the temperature of 0 ℃ is adopted as the circulating water; the alloy is melted by electric arc melting, the melted alloy material is stirred by high-speed electromagnetism, the electric arc current is closed rapidly after being maintained for 10 seconds, and the high-speed electromagnetism stirring is maintained for 5 seconds, so that the alloy is cooled rapidly. The alloy is rapidly quenched in a high-frequency heating single-roller rapid quenching furnace under the protection of argon, and the linear velocity of the surface of the wheel is 40 m/s. Then taking out the material obtained by quick quenching and carrying out vacuum annealing at 500 ℃ to obtain a cubic Laves single-phase compound. FIG. 2 shows Nd (Fe)0.6Co0.4)2The saturation magnetization of the alloy after the rapid quenching annealing is 58emu/g, and the insert of FIG. 3 shows Nd (Fe)0.6Co0.4)2The magnetostriction of the alloy after the rapid quenching annealing was 209 ppm.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A magnetostrictive material, characterized in that the magnetostrictive material comprises the following components: nd (Fe)1-xCox)2(ii) a Wherein x is 0.1 to 0.4.
2. The magnetostrictive material according to claim 1, characterized in that amorphous or amorphous and nanocrystalline mixture ribbons are obtained by melt rapid quenching and low temperature annealing to obtain cubic Laves single phase compounds.
3. A preparation process of a magnetostrictive material is characterized by comprising the following steps:
preparing raw materials: rare earth Nd and transition metals Fe and Co are adopted according to the stoichiometric formula Nd (Fe)1-xCox)2Proportioning by atomic ratio; wherein x is 0.1-0.4;
conventional vacuum arc melting: putting the metal simple substance obtained in the step into a copper crucible in a vacuum arc melting furnace cavity, closing the furnace cavity, pre-pumping by using a mechanical pump and continuously pumping by using a molecular pump until the vacuum degree in the furnace cavity reaches below 10-5Pa, and filling argon protective gas to the pressure of 0.06-0.09MPa lower than the atmospheric pressure; repeating the conventional smelting for 4 times until the alloy components are uniform;
quick cooling and smelting: changing the circulating water to an ice water mode, carrying out electric arc melting on the alloy to a molten state, carrying out high-speed electromagnetic stirring on the molten alloy material, maintaining for 10-20 seconds, quickly closing electric arc current, maintaining high-speed electromagnetic stirring for 5-10 seconds, and cooling the material to room temperature;
carrying out rapid quenching in a high-frequency heating single-roller rapid quenching furnace under the protection of argon;
and (3) vacuum annealing: and taking out the material and carrying out vacuum annealing to obtain the cubic Laves single-phase compound.
4. The process for preparing a magnetostrictive material according to claim 3, wherein the vacuum annealing temperature is 500-600 ℃.
5. The process according to claim 3, wherein the purity of Nd, Fe and Co is 99.9% or more.
6. The process of claim 3, wherein said conventional vacuum arc melting is performed by placing rare earth on lower transition metal and rare earth on upper transition metal.
7. The process for preparing a magnetostrictive material according to claim 3, wherein in the rapid quenching step, the linear velocity of the surface of the wheel is within the range of 20-45 m/s.
8. The process for preparing a magnetostrictive material according to claim 3, characterized in that the vacuum annealing is carried out for a period of more than 30 minutes.
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Citations (5)
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---|---|---|---|---|
CN1258757A (en) * | 1999-12-30 | 2000-07-05 | 南京大学 | Fast melt-quenching process to synthesize cubic laves phase giant magnetostrictive material with high Pr content |
CN1676650A (en) * | 2005-04-21 | 2005-10-05 | 南京大学 | Pr series rare earth super magnetostric tive material and its preparing method |
JP4771398B2 (en) * | 2004-05-26 | 2011-09-14 | Fdk株式会社 | Giant magnetostrictive thin film element and manufacturing method thereof |
CN103647019A (en) * | 2013-11-27 | 2014-03-19 | 南京航空航天大学 | Giant magnetostrictive material brewed via light rare earth and preparation technology of giant magnetostrictive material |
CN110423932A (en) * | 2019-08-23 | 2019-11-08 | 南京信息职业技术学院 | A kind of magnetostriction materials and preparation method of light rare earth Pr doping |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1258757A (en) * | 1999-12-30 | 2000-07-05 | 南京大学 | Fast melt-quenching process to synthesize cubic laves phase giant magnetostrictive material with high Pr content |
JP4771398B2 (en) * | 2004-05-26 | 2011-09-14 | Fdk株式会社 | Giant magnetostrictive thin film element and manufacturing method thereof |
CN1676650A (en) * | 2005-04-21 | 2005-10-05 | 南京大学 | Pr series rare earth super magnetostric tive material and its preparing method |
CN103647019A (en) * | 2013-11-27 | 2014-03-19 | 南京航空航天大学 | Giant magnetostrictive material brewed via light rare earth and preparation technology of giant magnetostrictive material |
CN110423932A (en) * | 2019-08-23 | 2019-11-08 | 南京信息职业技术学院 | A kind of magnetostriction materials and preparation method of light rare earth Pr doping |
Non-Patent Citations (2)
Title |
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C.C.HU: "Structural, magnetic and magnetostrictive behavior in Nd(Fe1-xCox)1.9 compounds", 《JOURNAL OF APPLIED PHYSICS》 * |
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