CN114807681A - Low-internal-consumption large-magnetostriction alloy and preparation method thereof - Google Patents
Low-internal-consumption large-magnetostriction alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-internal-consumption large-magnetostriction alloy and a preparation method thereof, wherein the material comprises the following components in percentage by weight: c: 0.02-0.05%, B: 0.007-0.015%, Ca: 0.002-0.01%, Mo: 0.10 to 0.99%, Nb: 1.0-2.0%, Ti: 3.1-4.0%, Al: 0.1-0.3%, Ni: 55.01-70.00%, and the balance Fe and inevitable impurities. The low-internal-consumption and large-magnetostriction alloy disclosed by the invention is simple and feasible in preparation method, low in internal consumption of the alloy and large in magnetostriction coefficient, effectively reduces the attenuation of elastic waves in a magnetostriction material, is applied to a magnetostriction sensor, and solves the technical problems of high signal attenuation, poor signal remote transmission performance and the like of the magnetostriction sensor produced in the prior art.
Description
Technical Field
The invention relates to an alloy, in particular to a magnetostrictive alloy material with low internal consumption and a preparation method thereof.
Background
The magnetostrictive material is a novel intelligent functional material which is rapidly developed in the sixty-seven years of the last century, has the function of converting electromagnetic energy and mechanical energy, is an important energy and information conversion functional material, and has wide application in the engineering fields of displacement measurement and control technology, ocean detection and development technology, micro-displacement driving, vibration reduction and prevention, noise reduction and prevention systems, intelligent wings, robots, automation technology, fuel injection technology microsensors, micro-vibrators, micromotors and the like. The magnetostrictive sensor prepared from the magnetostrictive material plays an increasingly important role in national economy and industrial production as a strategic material for improving the national high-tech comprehensive competitiveness in the 21 st century. Precision components such as magnetostrictive displacement sensors are increasingly developing towards large-range, high-precision and high-sensitivity directions, which puts higher requirements on the internal consumption and magnetostrictive performance of magnetostrictive alloys for precision components.
Internal losses, i.e. Q -1 And the value represents the attenuation degree of the energy of the harmonic oscillator in one vibration period. Under the same parameter condition, the saturation magnetostriction value lambda of the device s The larger the value, the larger the amplitude that can be maintained, which is more beneficial to improving the sensitivity of the device and reducing the noise level. When precise components such as a magnetostrictive displacement sensor work, signals generated by magnetostrictive materials in the magnetostrictive displacement sensor need to be transmitted for a long distance, and when the frequency temperature coefficient Q of the magnetostrictive materials -1 When the value is large, the elastic wave signal in the device can be greatly attenuated along with the change of the distance, so that the device can not work normally. Therefore, the magnetostrictive material must have a large λ at the same time s Value and low Q -1 The reliability and stability of the device can be ensured.
Among the several classes of magnetostrictive alloy materials available, Q of the material -1 The value is generally large, and the use requirement of a high-precision remote transmission sensor is difficult to meet. Q of most FeNi-based magnetostrictive material -1 The value is generally 3X 10 -3 ～5×10 -4 Q of FeCo, FeGa and FeAl-based highly magnetostrictive material -1 Values generally higher than 1X 10 -3 . Although the rare earth giant magnetostrictive material has an ultrahigh saturated magnetostrictive coefficient, the rare earth giant magnetostrictive material is large in brittleness, cannot be easily processed into a filament with a size required by a sensor, and cannot transmit signals caused by magnetostriction for a long distance due to excessive internal consumption. Having a small Q -1 Elastic alloys with values such as 3J33 are typically 1X 10 -4 ～4×10 -5 But the saturation magnetostriction coefficient is close to zero, and the magnetostriction effect is not generated. Therefore, there is a need to develop a magnetostriction film having a large magnetostriction property and a lower internal lossThe telescopic material is used for meeting the use requirement of high-precision components.
Disclosure of Invention
The invention aims to provide a magnetostrictive material with low internal consumption and large magnetostrictive coefficient and a manufacturing method thereof, which solve the problems of low sensitivity and poor remote transmission performance of a sensor caused by the fact that the conventional magnetostrictive material cannot have low internal consumption and large magnetostrictive coefficient. The material has a saturated magnetostriction coefficient lambda s of not less than 20 x 10 -6 Internal loss of Q -1 ≤1×10 -4 /° c, and has good processability.
The technical scheme of the invention is as follows:
the magnetostrictive alloy with low internal loss comprises the following components in percentage by weight: c: 0.02-0.05%, B: 0.007-0.015%, Ca: 0.002-0.01%, Mo: 0.10 to 0.99%, Nb: 1.0-2.0%, Ti: 3.1-4.0%, Al: 0.1-0.3%, Co: 1-2%, Ni: 55.01-70.00%, and the balance Fe and inevitable impurities.
The better technical scheme is that the alloy comprises the following components in percentage by weight: c: 0.03-0.05%, B: 0.007-0.009%, Ca: 0.002-0.004%, Mo: 0.60 to 0.93%, Nb: 1.3-1.6%, Ti: 3.2-3.5%, Al: 0.1 to 0.3%, Co: 1-2%, Ni: 55.1 to 60.00 percent, and the balance of Fe and inevitable impurities.
The impurities comprise the following components in percentage by weight: less than or equal to 0.002 percent of O, less than or equal to 0.1 percent of Si, less than or equal to 0.1 percent of Mn, less than or equal to 0.01 percent of S, less than or equal to 0.01 percent of P and less than or equal to 0.01 percent of Cr.
The preparation method of the alloy comprises the following steps:
1) taking the raw materials according to the proportion, carrying out vacuum melting, casting the raw materials into an electrode bar at 1500 ℃, and carrying out electroslag remelting after finishing to obtain an alloy steel ingot;
2) step 1), carrying out diffusion annealing on the alloy steel ingot at 1190-1210 ℃ for 2-8h to obtain a billet;
3) hot rolling:
step 2), hot rolling the billet at 900-1140 ℃ to roll the billet into a wire;
4) and (3) heat treatment:
step 3) continuously heat-treating the wire under the protection of hydrogen to obtain an alloy wire;
5) drawing
Step 4), drawing and reducing the alloy wire subjected to heat treatment to enable the size of the wire to be equal to that of the alloy wire
6) Electrolytic polishing and aging heat treatment
The method is characterized in that: step 3) the diameter of the wire is
The continuous heat treatment method in the step 4) comprises the following steps: (980-1070) and +/-5 ℃ for 0.5-2 hours.
And 5) performing electrolytic polishing on the reduced-diameter alloy wire rod obtained in the step 5), and then performing aging heat treatment in vacuum.
Polishing in the step 6), wherein the take-up speed is 0.05M/s, and the electrolyte is 5-15% of NaNO 3 +5～15％NaCl+H 2 And (4) O solution.
And 6) carrying out aging heat treatment, wherein the heat treatment system is 630-690 ℃, the temperature is kept for 3-5 hours, and the furnace cooling is carried out.
In the alloy of the present invention:
ni and Fe are used as basic elements of an austenite structure matrix formed by the alloy, have large magnetostriction performance and play a role in obtaining good cold and hot processing performance. Ni is effectively precipitated when alloying elements such as Ti, Al and Ni 3 The (TiAl) intermetallic compound strengthens the alloy, and precipitated phases are mutually wound and staggered with dislocations in a matrix, so that the movement of the dislocations is hindered, and the alloy has low internal consumption.
Mo and Nb initiate the action of the solid solution strengthening alloy, and a trace amount of C forms a fine carbide strengthening alloy with Ti, Nb, and the like.
Co can enter Ni 3 The (TiAl) intermetallic compound further strengthens the alloy, reduces the internal consumption of the alloy, and can also improve the Curie point of the alloy, thereby improving the service temperature of the alloy.
B. Ca strengthens the grain boundary and improves the alloy processability. The impurity elements such as O, S, Si, P, Cr, Mn, etc. are too high to adversely affect the internal loss and magnetostrictive property of the alloy, and are therefore strictly limited.
The properties of the alloy depend on the alloy components and also depend on the structure of the alloy, and the structure of the alloy is determined by the processes of smelting, hot rolling, cold working, heat treatment and the like of the alloy.
According to the invention, the purity of the alloy can be improved by vacuum induction melting and slag remelting, and the comprehensive performance of the alloy is improved; the diffusion annealing can reduce or eliminate cast dendrite segregation and avoid the formation of strip structure defects in the subsequent processing process of the alloy; uniform and fine grain structure can be obtained by hot rolling; through the cold drawing processing with large deformation, the positions with a large amount of precipitated phase nucleation in the alloy are ensured, the precipitated phases are finer and are uniformly dispersed, and the internal consumption of the alloy can be remarkably reduced while the alloy strengthening is promoted. By electrolytic polishing, the surface quality of the alloy material can be effectively improved, and the internal consumption of the alloy is further reduced; finally, an aging heat treatment process is adopted to precipitate intermetallic compound in the alloy in a dispersion way to strengthen the alloy.
The invention has the beneficial effects that:
1. the preparation method of the low-internal-consumption large-magnetostriction alloy is simple and convenient, short in preparation flow and low in preparation cost, and can be used for completing preparation through the working procedures of smelting, hot rolling, heat treatment, drawing and the like.
2. Through reasonable optimization design of alloy chemical components, the effects of all elements in the alloy are fully exerted, and the magnetostrictive alloy with low internal consumption and large magnetostrictive coefficient is prepared by combining the processes of vacuum induction melting, forging, hot rolling, heat treatment, drawing, electrolytic polishing and the like, so that the requirement of high-precision components on the alloy with low internal consumption and large magnetostrictive coefficient is met.
3. Applicants' experiments prove that the alloy of the invention has the saturated magnetostriction coefficient lambdas which is 22 multiplied by 10 -6 Internal loss Q -1 ＝8.9～9.3×10 -5 The alloy has very low internal loss and large saturated magnetostriction coefficient, effectively reduces the attenuation of signals in the magnetostriction material, and solves the problem of the magnetostriction material produced in the prior artFast signal attenuation, poor signal remote transmission performance and the like. Can be widely applied to various high-precision instruments and meters.
The preparation method of the low internal consumption large magnetostrictive alloy is simple and easy to implement, and the applicant tests and verifies that the saturated magnetostrictive coefficient lambdas of the low internal consumption large magnetostrictive alloy is 24-22 multiplied by 10 -6 Internal loss Q -1 ＝9.3-8.9×10 -5 The alloy has low internal consumption and large magnetostriction coefficient, effectively reduces the attenuation of elastic waves in the magnetostriction material, is applied to a magnetostriction sensor, and solves the technical problems of high signal attenuation, poor signal remote transmission performance and the like of the magnetostriction sensor produced in the prior art.
Drawings
FIG. 1 is a graph of the magnetostriction coefficient of the magnetostriction alloy material with low internal loss and large magnetostriction. DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
The preparation method of the low-internal-consumption large-magnetostriction alloy material comprises the following steps of preparing a copper-containing aluminum net for lightning protection from aluminum foil:
(1) pure nickel, pure iron, pure niobium and other raw materials are mixed according to the proportion of C: 0.03%, B: 0.008%, Ca: 0.003%, Mo: 0.69%, Nb: 1.6%, Ti: 3.4%, Al: 0.15%, Co: 1.63%, Ni: 55.1 percent and the balance of Fe are proportioned, vacuum induction smelted and cast into an electrode bar at 1500 ℃, and the electrode bar is subjected to electroslag remelting after surface finishing: electrode bar is slowly inserted into slag in molten state (slag ratio: CaF) 2 60％；Al 2 O 3 15.0 percent; 15% of CaO; 10% of MgO; ) After the arc is started, the voltage is regulated to be 42V and the current is regulated to be 3750A, and then the material melting is started. And (3) performing hot feeding shrinkage for 4 times before remelting, cooling the steel ingot in a crystallizer for 40 minutes after the hot feeding shrinkage is finished, and demolding to obtain the low-internal-consumption large-magnetostriction alloy electroslag ingot with the phi of 155 mm.
2) Carrying out diffusion annealing on the alloy steel ingot obtained in the step 1) at 1190 ℃ for 7 h;
3) hot rolling:
hot rolling the square billet obtained in the step 2) at 900-1140 ℃ to obtain the finished product
A wire rod;
4): and (3) heat treatment:
and (3) placing the hot-rolled wire rod in the hydrogen protection continuous heat treatment furnace, and preserving heat for 2 hours at 990 +/-5 ℃ to obtain the magnetostrictive alloy wire rod with excellent deformability.
5) Drawing
Drawing and reducing the alloy wire subjected to the heat treatment in the step 4) to prepare a wire with a required size, wherein the typical size is
6) Electrolytic polishing
Performing electrolytic polishing on the wire rod (low internal consumption large magnetostriction alloy wire rod) subjected to drawing and reducing by using direct current, wherein the polishing and take-up speed is 0.05M/s, and the electrolyte is 8% of NaNO 3 +7％NaCl+H 2 And (4) O solution.
7) Aging heat treatment
And (3) placing the low-internal-consumption large-magnetostriction alloy wire not in step 6) in a vacuum heat treatment furnace for aging heat treatment, wherein the heat treatment system is that the temperature is kept at 650 ℃ for 4 hours, and the wire is cooled along with the furnace to obtain the low-internal-consumption large-magnetostriction alloy (wire).
Measuring the saturation magnetostriction coefficient of the alloy by adopting a resistance strain effect; measuring and calculating the internal loss of the alloy by adopting a peak width method according to the GB/T15006 standard, wherein the saturated magnetostriction coefficient lambdas of the magnetostriction alloy with low internal loss and large magnetostriction prepared by adopting the method is 22 multiplied by 10 -6 Internal loss Q -1 ＝8.9×10 -5 /℃。
Example 2
Pure nickel, pure iron, pure niobium and other raw materials are mixed according to the proportion of C: 0.05%, B: 0.007%, Ca: 0.004%, Mo: 0.83%, Nb: 1.5%, Ti: 3.3%, Al: 0.11%, Co: 1.35%, Ni: 56.0 percent and the balance of Fe are proportioned, mixed, smelted in a vacuum induction mode, cast into an electrode bar at 1500 ℃, and subjected to electroslag remelting after the surface of the electrode bar is finished. The magnetostrictive alloy material with low internal consumption is prepared by the method of the embodiment 1.
Measuring the saturation magnetostriction coefficient of the alloy by adopting a resistance strain effect; and measuring and calculating the internal consumption of the alloy by adopting a peak width method according to the GB/T15006 standard. The saturation magnetostriction coefficient lambdas of the obtained low internal consumption giant magnetostriction alloy is 24 multiplied by 10 -6 Internal loss Q -1 ＝9.1×10 -5 /℃。
Example 3
Pure nickel, pure iron, pure niobium and other raw materials are mixed according to the proportion of C: 0.04%, B: 0.009%, Ca: 0.002%, Mo: 0.91%, Nb: 1.3%, Ti: 3.2%, Al: 0.17%, Co: 1.04%, Ni: 59.0 percent and the balance of Fe are proportioned, mixed, smelted by vacuum induction and cast into an electrode bar at 1500 ℃, and the electrode bar is subjected to electroslag remelting after surface finishing. The magnetostrictive alloy material with low internal consumption is prepared by the method of the embodiment 1.
Measuring the saturation magnetostriction coefficient of the alloy by adopting a resistance strain effect; and measuring and calculating the internal consumption of the alloy by adopting a peak width method according to the GB/T15006 standard. The saturation magnetostriction coefficient lambdas of the obtained low internal loss giant magnetostriction alloy is 22 multiplied by 10 -6 Internal loss Q -1 ＝9.3×10 -5 /℃。
Example 4
Pure nickel, pure iron, pure niobium and other raw materials are mixed according to the proportion of C: 0.035%, B: 0.008%, Ca: 0.003%, Mo: 0.64%, Nb: 1.45%, Ti: 3.37%, Al: 0.13%, Co: 1.29%, Ni: 56.8 percent and the balance of Fe are proportioned, mixed, smelted in a vacuum induction mode, cast into an electrode bar at 1500 ℃, and subjected to electroslag remelting after the surface of the electrode bar is finished. The magnetostrictive alloy material with low internal consumption is prepared by the method of the embodiment 1.
Measuring the saturation magnetostriction coefficient of the alloy by adopting a resistance strain effect; and measuring and calculating the internal consumption of the alloy by adopting a peak width method according to the GB/T15006 standard. The saturation magnetostriction coefficient lambdas of the obtained low internal loss giant magnetostriction alloy is 23 × 10 -6 Internal loss Q -1 ＝8.9×10 -5 /℃。
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (9)
1. The magnetostrictive alloy with low internal loss is characterized by comprising the following components in percentage by weight: c: 0.02-0.05%, B: 0.007-0.015%, Ca: 0.002-0.01%, Mo: 0.10 to 0.99%, Nb: 1.0-2.0%, Ti: 3.1-4.0%, Al: 0.1-0.3%, Co: 1-2%, Ni: 55.01-70.00%, and the balance Fe and inevitable impurities.
2. The alloy of claim 1, wherein the alloy comprises the following components in weight percent: c: 0.03-0.05%, B: 0.007-0.009%, Ca: 0.002-0.004%, Mo: 0.60 to 0.93%, Nb: 1.3-1.6%, Ti: 3.2-3.5%, Al: 0.1-0.3%, Co: 1.0-1.8%, Ni: 55.1 to 60.00 percent, and the balance of Fe and inevitable impurities.
3. The alloy of claim 1 or 2, wherein the impurities comprise, in weight percent: less than or equal to 0.002 percent of O, less than or equal to 0.1 percent of Si, less than or equal to 0.1 percent of Mn, less than or equal to 0.01 percent of S, less than or equal to 0.01 percent of P and less than or equal to 0.01 percent of Cr.
4. A method of making the alloy of claim 1, comprising the steps of:
1) taking the raw materials according to the proportion of claim 1 or 2, vacuum melting, casting into an electrode bar at 1500 ℃, and remelting electroslag after finishing to obtain an alloy steel ingot;
2) step 1), carrying out diffusion annealing on the alloy steel ingot at 1190-1210 ℃ for 2-8h to obtain a billet;
3) hot rolling:
step 2), hot rolling the billet at 900-1140 ℃ to roll the billet into a wire;
4) and (3) heat treatment:
step 3) continuously heat-treating the wire under the protection of hydrogen to obtain an alloy wire;
5) drawing
Step 4), drawing and reducing the alloy wire subjected to heat treatment until the size of the wire is
6) Electrolytic polishing and aging heat treatment.
5. The method according to claim 4, wherein: step 3) the diameter of the wire is
6. The method according to claim 4, wherein: the continuous heat treatment method in the step 4) comprises the following steps: (980-1070) and +/-5 ℃ for 0.5-2 hours.
7. The method according to claim 4, wherein: and 5) performing electrolytic polishing on the reduced-diameter alloy wire rod obtained in the step 5), and then performing aging heat treatment in vacuum.
8. The method according to claim 4, wherein: the polishing in the step 6) has the take-up speed of 0.05M/s and the electrolyte of 5-15 percent NaNO 3 +5～15％NaCl+H 2 And (4) O solution.
9. The method according to claim 4, wherein: and 6) carrying out aging heat treatment, wherein the heat treatment system is 630-690 ℃, the temperature is kept for 3-5 hours, and the furnace cooling is carried out.
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| US4566917A (en) * | 1980-03-25 | 1986-01-28 | Allied Corporation | Low magnetostriction amorphous metal alloys |
| CN102867608A (en) * | 2012-08-29 | 2013-01-09 | 苏州宝越新材料科技有限公司 | FeNi-based amorphous soft magnetic alloy and preparation method of soft magnetic alloy |
| CN103556071A (en) * | 2013-11-21 | 2014-02-05 | 重庆材料研究院有限公司 | High temperature radiation resistant magnetostriction alloy |
| CN103556005A (en) * | 2013-11-21 | 2014-02-05 | 重庆材料研究院有限公司 | High temperature FeNiCo magnetostriction alloy as well as preparation method thereof |
| CN104946955A (en) * | 2015-06-26 | 2015-09-30 | 西安理工大学 | Fe-Ni metal-based magnetostrictive material and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4566917A (en) * | 1980-03-25 | 1986-01-28 | Allied Corporation | Low magnetostriction amorphous metal alloys |
| CN102867608A (en) * | 2012-08-29 | 2013-01-09 | 苏州宝越新材料科技有限公司 | FeNi-based amorphous soft magnetic alloy and preparation method of soft magnetic alloy |
| CN103556071A (en) * | 2013-11-21 | 2014-02-05 | 重庆材料研究院有限公司 | High temperature radiation resistant magnetostriction alloy |
| CN103556005A (en) * | 2013-11-21 | 2014-02-05 | 重庆材料研究院有限公司 | High temperature FeNiCo magnetostriction alloy as well as preparation method thereof |
| CN104946955A (en) * | 2015-06-26 | 2015-09-30 | 西安理工大学 | Fe-Ni metal-based magnetostrictive material and preparation method thereof |
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