High-performance iron-based magnetostrictive alloy sheet and method of manufacturing

Abstract

The application provides a high-performance iron-based magnetostrictive alloy sheet and a preparation method, and belongs to the technical field of magnetic functional materials. The high-performance iron-based magnetostrictive alloy sheet material is composed of (Fe 1‑x‑z Ga x Al y Cr z ) 100‑a‑b M a N b , wherein x=0.1-0.3, y=0.0-0.1, z=0.0-0.05, a=0.01-1.0, b=0.01-0.5, M is one or more of B, Nb, C, Ti, V, Mn, N and S, and N is one or more of La, Ce, Pr, Nd, Sm, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr. The preparation method is used for preparing the high-performance iron-based magnetostrictive alloy sheet with improved magnetostrictive performance through raw material pretreatment, proportioning and weighing of raw materials, alloy billet preparation, hot forging, hot rolling+warm rolling+cold rolling and three-stage temperature rising heat treatment+(Tb / Dy)Cu diffusion heat treatment. The method is simple in process and easy to operate, low in cost and high in efficiency, the prepared product is small in eddy current loss, wide in applicable frequency demand, and is beneficial to industrial large-scale production and application promotion.

Description

Technical Field

[0001] This invention relates to the technical field of magnetic functional materials, specifically to a high-performance iron-based magnetostrictive alloy thin plate and its preparation method. Background Technology

[0002] When the magnetization state of ferromagnetic and subferromagnetic materials changes, their length and volume undergo minute changes; this phenomenon is called magnetostriction. The change in volume is called volumetric magnetostriction, and the change in length is called linear magnetostriction. Practical magnetostrictive materials refer to linear magnetostrictive materials, and their properties are characterized by the magnetostriction coefficient λ, where λ = ΔL / L (L is the original length of the material, and ΔL is the change in the sample when the magnetization state changes).

[0003] Traditional magnetostrictive materials include pure Ni, Ni-based alloys, Fe-based alloys, and ferrite materials. The magnetostriction coefficient of polycrystalline pure Ni is between 35 and 40 ppm (1 ppm = 10⁻⁶). -6 Practical Ni-based and Fe-based alloys exhibit magnetostriction below 100 ppm; ferrites typically have a magnetostriction coefficient between 10 and 50 ppm. Magnetostrictive materials, as a type of transducer, have been used in transducer technology since the 1940s and 50s. Because magnetostriction can generate significant forces with a short response time, magnetostrictive materials have also found applications in actuation, sensing, and other technological fields.

[0004] As intelligent agents capable of sensing, interacting, and performing tasks in the physical world, embodied robots face urgent demands for high precision, high response, high reliability, and miniaturization in their core components. Magnetostrictive materials (such as Terfenol-D and Galfenol) exhibit significant application potential in this industry due to their unique physical properties. Key requirements include: high-precision sensing and feedback; high-speed, high-precision micro-actuators and positioning; compact structures and lightweight designs; resistance to harsh environments and high reliability; and energy recovery and self-powering potential. The core demand for magnetostrictive materials in the embodied robot industry lies in their ability to fill the gaps in precision, response speed, and environmental adaptability inherent in traditional sensing and actuation technologies. With decreasing material costs, optimized processes, and deep integration with intelligent control algorithms, magnetostrictive technology is expected to become a key enabling factor in improving the dynamic performance and environmental interaction capabilities of robots.

[0005] In the 1980s, Clark et al. in the United States invented a magnetostrictive material (Terfenol-D) composed of rare earth elements and Fe, called rare earth supermagnetostrictive material. Rare earth supermagnetostrictive materials possess very high magnetostriction coefficients. The magnetostriction coefficient of single-crystal rare earth supermagnetostrictive materials reaches as high as 2000 ppm; the magnetostriction coefficient of polycrystalline rare earth supermagnetostrictive materials can reach 1000-1500 ppm under a magnetic field of 80 kA / m and a certain pre-stress. Due to the large strain and low Young's modulus characteristics of polycrystalline rare earth supermagnetostrictive materials, this material has been well applied in the field of underwater acoustic transduction. However, the main phase of polycrystalline rare earth supermagnetostrictive materials is a Laves phase intermetallic compound, which is intrinsically brittle and has very high electrical conductivity. When used at higher frequencies, eddy current losses can severely affect its energy output or displacement output.

[0006] In 2000, Guruswamy S et al. in the United States reported a binary alloy composed of Fe and Ga, namely FeGa alloy (Galfenol), which has a high λ value, as well as advantages such as high strength, low brittleness, very low saturation magnetization field, and high magnetic permeability. It is a new type of magnetostrictive material.

[0007] A 2003 study by Kellogg et al. showed that Fe 83 Ga 17 The tensile strength of the alloy can reach 450 MPa. In the same year, the Japan Institute of Metals prepared a Fe-Ga alloy rapid solidification thin strip sample with a large magnetostrictive strain value of 400 ppm, and it did not break even after bending 180°, exhibiting good ductility. However, the main preparation methods for Fe-Ga alloys currently in use are: a. directional solidification; b. rapid quenching of thin strips; c. bonding and other powder metallurgy methods. Materials prepared by these methods all have various defects. FeGa-based magnetostrictive alloys prepared by directional solidification have low resistivity and are prone to high-frequency eddy current losses, which limits their use in high-frequency fields. While composite materials prepared by bonding methods can overcome the problem of high-frequency eddy current losses, their magnetostrictive properties are much lower, and the material itself has low strength. In practical applications, to avoid heat generation and material failure due to eddy current losses, FeGa-based magnetostrictive alloys are usually processed into thin sheets or strips; as the material thickness decreases, the eddy current loss also decreases. The strips produced by the rapid quenching method are small in size and only exhibit excellent magnetostrictive properties when subjected to an external strong magnetic field. The overall material properties are poor and there are currently no practical applications.

[0008] Chinese patent CN101465406A discloses a high-performance polycrystalline textured Fe-Ga-based magnetostrictive sheet material and its preparation method. However, due to the presence of oxygen or hydrogen sulfide gas during atmospheric heat treatment, the stability of the surface energy-induced texture formation is difficult to control along the rolling direction. <001> It suffers from numerous technical defects, such as weak texture strength and poor magnetostrictive properties.

[0009] Chinese patent CN103014594A discloses a method for preparing high-performance magnetostrictive thin strips. In this technology, the surface of the strip is decomposed by solid sulfur or hydrogen sulfide gas to adsorb sulfur elements to reduce the surface energy, thereby inducing the formation of texture. However, the sulfur elements need to be removed by heat treatment in a reducing atmosphere in the later stage. Therefore, there are many technical defects such as complex heat treatment process and easy residue of sulfur elements that deteriorate mechanical properties.

[0010] Chinese patent CN101654759A discloses a method for preparing Fe-Ga-Al based sheet magnetostrictive materials from Fe-Ga-Al based raw materials. However, this technique suffers from limitations in the preparation process that cannot impart strong magnetic properties along the rolling direction to the final sheet. <001> Due to its texture, it suffers from the technical defect of low magnetostrictive performance. Summary of the Invention

[0011] The main objective of this invention is to address the technical problems of insufficient texture control stability and low mechanical and magnetostrictive properties in existing magnetostrictive alloy thin sheet technology. Therefore, this invention provides a high-performance iron-based magnetostrictive alloy thin sheet and its preparation method, resulting in a high-performance iron-based magnetostrictive alloy thin sheet material with high magnetostriction coefficient, good mechanical processing properties, and the ability to meet plastic processing requirements.

[0012] The technical solution is as follows:

[0013] A high-performance iron-based magnetostrictive alloy sheet, wherein the thickness of the high-performance iron-based magnetostrictive alloy sheet is 0.05-0.5 mm, and the composition is (Fe 1-x-z Ga x Al y Cr z ) 100-a-b M a N b , where x=0.1-0.3, y=0.0-0.1, z=0.0-0.05, a=0.01-1.0, b=0.01-0.5, M is one or more of B, Nb, C, Ti, V, Mn, N and S, and N is one or more of La, Ce, Pr, Nd, Sm, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr.

[0014] Optionally, the high-performance iron-based magnetostrictive alloy sheet will acquire a strong Gaussian texture or cubic texture along the rolling direction. One or more of the elements N, La, Ce, Pr, Nd, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing clusters of locally ordered structures.

[0015] Optionally, the density of the high-performance iron-based magnetostrictive alloy sheet is 7.52-7.91 g / cm³. 3 The hardness is 213-242 HV, the tensile strength is 410-720 MPa, and the elongation is 2-5%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 150-230 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 350-390 ppm. The Curie temperature is >650℃, the saturation magnetic induction intensity is 1.44-1.68 T, and the resistivity is 83 × 10⁻⁶. -8 -96×10 -8 Ω·cm, relative permeability 72-109, coercivity Hc 89-126 A / m.

[0016] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0017] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0018] S2. Weighing and proportioning of raw materials: Weigh and proportion the pre-treated raw materials according to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet in S1. The proportion needs to take into account the burning loss to obtain the prepared raw materials.

[0019] S3. Alloy billet preparation: The raw materials prepared in S2 are smelted in a vacuum induction furnace, magnetic levitation furnace or electric arc melting furnace to obtain an alloy billet with uniform composition.

[0020] S4. Hot forging: After high-temperature homogenization annealing, the alloy billet with uniform composition of S3 is hot forged to obtain alloy forging material.

[0021] S5, hot rolling + warm rolling + cold rolling: hot rolling + warm rolling + cold rolling of S4 alloy forgings to obtain iron-based magnetostrictive alloy thin plates;

[0022] S6, Three-stage heating heat treatment + (Tb / Dy)Cu diffusion heat treatment: The iron-based magnetostrictive alloy sheet of S5 is subjected to three-stage heating heat treatment after rolling + (Tb / Dy)Cu diffusion heat treatment to obtain the finished iron-based magnetostrictive alloy sheet.

[0023] Optionally, the burn-off in S2 includes volatile elements such as Ga and Mn, with a burn-off amount of 2-5%.

[0024] Optionally, in S3 smelting, a vacuum is first applied to 10... -3 -10 -2 Argon gas at 400 Pa is then introduced and heated to melt the raw materials and form an alloy. After melting, the alloy is refined for 2-3 minutes to ensure the uniformity of the alloy composition. The refined alloy is then cast into alloy ingots or prepared into alloy rods through directional solidification.

[0025] Alternatively, the smelting process in S3 can be implemented using one of the following two methods:

[0026] Method 1: According to the alloy composition ratio, and with the addition of an appropriate amount of burn-off, the alloy is induction or arc melted under argon protection until completely homogeneous, and then cast into an alloy ingot. The alloy structure is non-oriented equiaxed crystal.

[0027] Method 2: According to the alloy composition ratio, and with the addition of an appropriate amount of slag, induction melting is carried out under argon protection until completely homogeneous. Then, directional solidification is performed. The growth direction of columnar crystals is controlled by the pulling rate to obtain a product with… <110> or <100> Oriented columnar crystal structure, with a pulling rate of 0.01-30 mm / min.

[0028] Optionally, the temperature for high-temperature homogenization annealing in S4 is 920-1050℃, and the holding time is 5-10h; the temperature for hot forging is 900-1100℃, the deformation per heat is controlled at 5-10%, and the total deformation is 50-70%.

[0029] Optionally, S5 can be hot-rolled + warm-rolled + cold-rolled. The initial rolling temperature of hot rolling is 900-1250℃, with 5-10 rolling passes, a reduction of 3-10% per pass, and a total reduction of 50-95%. The final rolling temperature is not lower than 830℃, and the hot-rolled plate is air-cooled to room temperature. The rolling temperature of warm rolling is 300-500℃, with 10-20 rolling passes, a reduction of 2-5% per pass, and a total reduction of 50-95%. The warm-rolled plate is air-cooled to room temperature after pickling. The warm-rolled plate is then cold-rolled at room temperature with 15-30 rolling passes, a reduction of 1-3% per pass, and a total reduction of 50-90%. The thickness of the iron-based magnetostrictive alloy sheet is between 0.05-0.5mm.

[0030] Optionally, in S6, the heat treatment is carried out under the protection of a flowing atmosphere containing ammonia, wherein the flowing atmosphere is argon or a mixture of nitrogen and argon, wherein the volume ratio of nitrogen in the mixture is less than 50%, and the volume ratio of ammonia in the flowing atmosphere is 5-20%.

[0031] Optionally, the three-stage heating heat treatment and (Tb / Dy)Cu diffusion heat treatment in S6 are as follows: from room temperature to the initial recrystallization temperature of 780-880℃, the heating rate is 5-10℃ / min, and the holding time is 5-15min; from the initial recrystallization temperature to the secondary recrystallization start temperature of 780-950℃, the heating rate is 20-40℃ / min, and the holding time is not maintained; from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 900-1250℃, the heating rate is 0.01-3℃ / min, and the holding time is maintained for 2-10h after the heating is completed, and then the temperature is air-cooled to room temperature after the holding time is completed.

[0032] The diffusion heat treatment of (Tb / Dy)Cu is as follows: heat to 1250-1350℃ at a heating rate of 5-20℃ / min, hold for 2-4 hours, and then cool to room temperature by water quenching or brine quenching.

[0033] Technical principle of the invention:

[0034] Plastic forming of metals is a processing method that causes metals to undergo plastic deformation under external force to obtain products with desired shapes, dimensions, and microstructures. Utilizing metal plastic forming techniques such as rolling not only yields workpieces with high strength, good performance, complex shapes, and high precision, but also offers advantages such as high productivity and low material consumption. Therefore, it is the mainstream process for preparing FeGa-based magnetostrictive alloy sheets or strips.

[0035] This invention, through compositional design of FeGa-based magnetostrictive alloys and the use of specific heat treatment processes, ultimately obtains alloy thin plates with macroscopically strong Gaussian or cubic textures and grain sizes reaching several centimeters, and microscopically exhibiting a disordered matrix containing locally ordered structural clusters, among other cross-scale structural features. The magnetostrictive performance (3 / 2)λs of the alloy thin plates can reach over 350 ppm, approaching or reaching the level of single-crystal FeGa alloys with trace amounts of heavy rare earth elements.

[0036] The material obtained by this invention has good magnetostrictive properties and good mechanical processing properties. It can be directly molded into products through relatively simple plastic processing, which can greatly save costs and is expected to be applied in many fields such as aviation, aerospace, navigation, androids, and energy.

[0037] The above technical solution has at least the following advantages compared with the existing technology:

[0038] The present invention proposes a high-performance iron-based magnetostrictive alloy thin plate and its preparation method, which solves the technical problems of insufficient texture control stability, low mechanical properties and magnetostrictive properties in existing magnetostrictive alloy thin plate technology.

[0039] This invention employs the principle of "organic inheritance" based on initial orientation, combined with the principle of inducing abnormal grain growth by using finely dispersed second-phase precipitation (carbide, nitride, carbonitride, or rare-earth-rich precipitates) and surface energy regulation. By controlling the heat treatment process (temperature, time, atmosphere, heating and cooling rates, diffusion heat treatment, and final cooling rate, etc.), a macroscopic structure with strong Gaussian or cubic texture and grain size reaching several centimeters is obtained, similar to a single-crystal structure, which is beneficial for improving magnetostrictive properties.

[0040] This invention is based on the principle of "nano-heterogeneous structure". After a thin plate has undergone three-stage heating heat treatment, it is subjected to (Tb / Dy)Cu diffusion heat treatment. The plate is heated to 1250-1350℃ and held for 2-4 hours, followed by water quenching or salt water quenching to room temperature. This forces one or more elements such as La, Ce, Pr, Nd, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr to dissolve in the alloy matrix. This induces locally ordered structures or structural clusters (B2-like or M-DO3 or L60 structures) in the disordered A2 structure of the matrix. Microscopically, this forms a microstructure feature of disordered matrix containing locally ordered structural clusters, which further improves the magnetostrictive properties of the alloy thin plate.

[0041] The high-performance iron-based magnetostrictive alloy thin sheet prepared by the method of this invention has a density of 7.52-7.91 g / cm³. 3 The hardness is 213-242 HV, the tensile strength is 410-720 MPa, and the elongation is 2-5%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 150-230 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 350-390 ppm. The Curie temperature is >650℃, the saturation magnetic induction intensity is 1.44-1.68 T, and the resistivity is 83 × 10⁻⁶. -8 -96×10 -8 Ω·cm, relative permeability 72-109, coercivity Hc 89-126 A / m.

[0042] The high-performance iron-based magnetostrictive alloy sheet of the present invention has a thickness between 0.05-0.5 mm, low eddy current loss, and can be applied to different frequency requirements.

[0043] The material preparation process of this invention is not demanding, has low cost, and is conducive to widespread application.

[0044] In summary, compared with the magnetostrictive alloy sheet technology, the method of this invention prepares high-performance iron-based magnetostrictive alloy sheets with improved magnetostrictive properties through raw material pretreatment, raw material proportioning and weighing, alloy billet preparation, hot forging, hot rolling + warm rolling + cold rolling, and three-stage heating heat treatment + (Tb / Dy)Cu diffusion heat treatment. This method is simple in process, easy to operate, low in cost, and high in efficiency. The prepared products have low eddy current loss and are applicable to a wide range of frequencies, which is conducive to large-scale industrial production and application. Attached Figure Description

[0045] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0046] Figure 1 This is a high-performance iron-based magnetostrictive (Fe) product according to Embodiment 1 of the present invention. 0.8 Ga 0.16 Al 0.02 Cr 0.02 ) 99.87 (NbC) 0.1 Tb 0.03 Magnetostrictive property curves of alloy thin sheets;

[0047] Figure 2 This is a high-performance iron-based magnetostrictive (Fe) product according to Embodiment 2 of the present invention. 0.8 Ga 0.16 Al 0.04 ) 99.75 B 0.2 Nd 0.05 Magnetostrictive property curves of alloy thin sheets;

[0048] Figure 3 This is a high-performance iron-based magnetostrictive (Fe) product according to Embodiment 3 of the present invention. 0.8 Ga 0.17 ) 99.75 Mn 0.1 (TiC) 0.1 Ho 0.05 Magnetostrictive property curve of alloy sheet. Detailed Implementation

[0049] The technical solution of the present invention will now be described with reference to the accompanying drawings.

[0050] In embodiments of the present invention, words such as "exemplarily," "for example," etc., are used to indicate that something is an example, illustration, or description. Any embodiment or design described as "exemplary" in the present invention should not be construed as being more preferred or advantageous than other embodiments or designs. Specifically, the use of the word "exemplary" is intended to present the concept in a concrete manner. Furthermore, in embodiments of the present invention, the meaning expressed by "and / or" can be both, or either one.

[0051] In the embodiments of the present invention, the terms "image" and "picture" may sometimes be used interchangeably. It should be noted that when the distinction is not emphasized, their intended meanings are consistent.

[0052] In this embodiment of the invention, sometimes a subscript such as W1 may be written in a non-subscript form such as W1. When the difference is not emphasized, the meaning they express is the same.

[0053] To make the technical problems, technical solutions and advantages of the present invention clearer, a detailed description will be given below in conjunction with the accompanying drawings and specific embodiments.

[0054] A high-performance iron-based magnetostrictive alloy sheet, wherein the thickness of the high-performance iron-based magnetostrictive alloy sheet is 0.05-0.5 mm, and the composition is (Fe 1-x-z Ga x Al y Cr z ) 100-a-b M a N b , where x=0.1-0.3, y=0.0-0.1, z=0.0-0.05, a=0.01-1.0, b=0.01-0.5, M is one or more of B, Nb, C, Ti, V, Mn, N and S, and N is one or more of La, Ce, Pr, Nd, Sm, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr.

[0055] In particular, the high-performance iron-based magnetostrictive alloy sheet will acquire a strong Gaussian texture or cubic texture along the rolling direction. One or more of the elements N, La, Ce, Pr, Nd, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing clusters of locally ordered structures.

[0056] Specifically, the density of the high-performance iron-based magnetostrictive alloy sheet is 7.52-7.91 g / cm³. 3The hardness is 213-242 HV, the tensile strength is 410-720 MPa, and the elongation is 2-5%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 150-230 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 350-390 ppm. The Curie temperature is >650℃, the saturation magnetic induction intensity is 1.44-1.68 T, and the resistivity is 83 × 10⁻⁶. -8 -96×10 -8 Ω·cm, relative permeability 72-109, coercivity Hc 89-126 A / m.

[0057] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0058] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0059] S2. Weighing and proportioning of raw materials: Weigh and proportion the pre-treated raw materials according to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet in S1. The proportion needs to take into account the burning loss to obtain the prepared raw materials.

[0060] S3. Alloy billet preparation: The raw materials prepared in S2 are smelted in a vacuum induction furnace, magnetic levitation furnace or electric arc melting furnace to obtain an alloy billet with uniform composition.

[0061] S4. Hot forging: The alloy casting billet with uniform composition of S3 is subjected to high-temperature homogenization annealing and then hot forging to obtain alloy forging material.

[0062] S5, hot rolling + warm rolling + cold rolling: hot rolling + warm rolling + cold rolling of S4 alloy forgings to obtain iron-based magnetostrictive alloy thin plates;

[0063] S6, Three-stage heating heat treatment + (Tb / Dy)Cu diffusion heat treatment: The iron-based magnetostrictive alloy sheet of S5 is subjected to three-stage heating heat treatment after rolling + (Tb / Dy)Cu diffusion heat treatment to obtain the finished iron-based magnetostrictive alloy sheet.

[0064] In particular, the burn-off in S2 includes volatile elements such as Ga and Mn, with a burn-off rate of 2-5%.

[0065] Specifically, in the S3 smelting process, a vacuum of 10 is first applied. -3 -10 -2Argon gas at 400 Pa is then introduced and heated to melt the raw materials and form an alloy. After melting, the alloy is refined for 2-3 minutes to ensure the uniformity of the alloy composition. The refined alloy is then cast into alloy ingots or prepared into alloy rods through directional solidification.

[0066] Specifically, the smelting process in S3 is implemented using one of the following two methods:

[0067] Method 1: According to the alloy composition ratio, and with the addition of an appropriate amount of burn-off, the alloy is induction or arc melted under argon protection until completely homogeneous, and then cast into an alloy ingot. The alloy structure is non-oriented equiaxed crystal.

[0068] Method 2: According to the alloy composition ratio, and with the addition of an appropriate amount of slag, induction melting is carried out under argon protection until completely homogeneous. Then, directional solidification is performed. The growth direction of columnar crystals is controlled by the pulling rate to obtain a product with… <110> or <100> Oriented columnar crystal structure, with a pulling rate of 0.01-30 mm / min.

[0069] Specifically, the high-temperature homogenization annealing temperature in S4 is 920-1050℃, and the holding time is 5-10h; the hot forging temperature is 900-1100℃, the deformation per heat is controlled at 5-10%, and the total deformation is 50-70%.

[0070] Specifically, S5 involves hot rolling + warm rolling + cold rolling. The initial rolling temperature for hot rolling is 900-1250℃, with 5-10 rolling passes, a reduction of 3-10% per pass, and a total reduction of 50-95%. The final rolling temperature is not lower than 830℃, and the hot-rolled sheet is air-cooled to room temperature. The warm rolling temperature is 300-500℃, with 10-20 rolling passes, a reduction of 2-5% per pass, and a total reduction of 50-95%. The warm-rolled sheet is air-cooled to room temperature after pickling. The warm-rolled sheet is then cold-rolled at room temperature with 15-30 rolling passes, a reduction of 1-3% per pass, and a total reduction of 50-90%. The thickness of the iron-based magnetostrictive alloy sheet is between 0.05-0.5mm.

[0071] Specifically, in S6, the heat treatment is carried out under the protection of a flowing atmosphere containing ammonia, and the flowing atmosphere is argon or a mixture of nitrogen and argon, wherein the volume ratio of nitrogen in the mixture is less than 50% and the volume ratio of ammonia in the flowing atmosphere is 5-20%.

[0072] Specifically, the three-stage heating heat treatment and (Tb / Dy)Cu diffusion heat treatment in S6 are as follows: from room temperature to the initial recrystallization temperature of 780-880℃, the heating rate is 5-10℃ / min, and the holding time is 5-15min; from the initial recrystallization temperature to the secondary recrystallization start temperature of 780-950℃, the heating rate is 20-40℃ / min, and the holding time is not maintained; from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 900-1250℃, the heating rate is 0.01-3℃ / min, and the holding time is 2-10h after the heating is completed, and then the temperature is air-cooled to room temperature after the holding time is completed.

[0073] The diffusion heat treatment of (Tb / Dy)Cu is as follows: heat to 1250-1350℃ at a heating rate of 5-20℃ / min, hold for 2-4 hours, and then cool to room temperature by water quenching or brine quenching.

[0074] Example 1

[0075] This embodiment describes a high-performance iron-based magnetostrictive alloy sheet, wherein the thickness of the high-performance iron-based magnetostrictive alloy sheet is 0.32 mm, and the composition is (Fe 0.8 Ga 0.16 Al 0.02 Cr 0.02 ) 99.87 (NbC) 0.1 Tb 0.03 .

[0076] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0077] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0078] S2. Raw material proportioning and weighing: According to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet, the raw materials for the pretreatment in S1 are weighed and proportioned. The proportioning needs to take into account the burning loss, which includes Ga burning loss, and the burning loss is 5%, to obtain the prepared raw materials. The prepared raw materials include Fe, Ga, Al and Cr with a purity greater than 99.9%, rare earth element Tb with a purity greater than 99.99%, and Nb and C are added in the form of NbFe and Fe-C master alloys, respectively.

[0079] S3. Alloy billet preparation: The raw materials prepared in S2 are evacuated in a vacuum induction furnace and then filled with Ar as a protective gas. The furnace is induction heated until completely melted, refined for 3 minutes, and then cast to obtain an alloy billet with uniform composition.

[0080] S4. Hot forging: The alloy billet with uniform composition of S3 is homogenized and annealed at 920℃ for 6 hours, and then hot forged into a slab. The hot forging temperature is 950℃, the deformation per hot forging is controlled at 8%, and the total deformation is 60%, to obtain alloy forging material.

[0081] S5. Hot rolling + warm rolling + cold rolling: The S4 alloy forging is subjected to hot rolling + warm rolling + cold rolling. The initial rolling temperature of hot rolling is 1020℃, with 8 rolling passes, a reduction of 8% per pass, and a total reduction of 64%. The final rolling temperature is not lower than 830℃. After hot rolling, it is air-cooled to room temperature. The rolling temperature of warm rolling is 480℃, with 18 rolling passes, a reduction of 4% per pass, and a total reduction of 72%. After warm rolling, it is air-cooled to room temperature. After pickling, the warm-rolled plate is cold-rolled at room temperature with 28 rolling passes, a reduction of 2% per pass, and a total reduction of 56%, to obtain a 0.32mm thick iron-based magnetostrictive alloy sheet.

[0082] S6. Three-stage heating heat treatment + DyCu diffusion heat treatment: The three-stage heating heat treatment of the iron-based magnetostrictive alloy sheet after rolling of S5 needs to be carried out in an ammonia-argon-nitrogen mixed atmosphere (ammonia volume ratio of 10% and nitrogen volume ratio of 30%). First, the temperature is raised from room temperature to the initial recrystallization temperature of 820℃ at a heating rate of 5℃ / min and held for 7min. Then, the temperature is raised from the initial recrystallization temperature to the secondary recrystallization start temperature of 920℃ at a heating rate of 20℃ / min without holding. After that, the temperature is raised from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 1150℃ at a heating rate of 0.85℃ / min. The flowing atmosphere is changed to pure argon. After the heating is completed, the temperature is held for 4h. After the holding is completed, the temperature is air-cooled to room temperature.

[0083] Then, a DyCu diffusion heat treatment was performed to create a DyCu layer with a thickness of approximately 20-30 μm. 0.6 Cu 0.4 The alloy rapid quenching strip is spread on both sides of the thin plate, and the temperature is raised to 1250℃ at a heating rate of 10℃ / min. After holding at this temperature for 2 hours, it is quenched in salt water and cooled to room temperature to obtain the finished iron-based magnetostrictive alloy thin plate.

[0084] The high-performance iron-based magnetostrictive alloy sheet prepared in this embodiment will have a strong Gaussian texture or cubic texture along the rolling direction. Tb and Dy are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing a cluster of locally ordered structures.

[0085] The high-performance iron-based magnetostrictive (Fe) prepared in this embodiment 0.8 Ga 0.16 Al 0.02 Cr 0.02 ) 99.87 (NbC)0.1 Tb 0.03 The density of the finished alloy sheet is 7.78 g / cm³. 3 It has a hardness of 241HV, a tensile strength of 468MPa, and an elongation of 4.6%; Figure 1 As shown, under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 223 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 362 ppm; the Curie temperature is 686℃, the saturation magnetic induction is 1.56 T, and the resistivity is 86 × 10⁻⁶. -8 It has a strength of Ω·cm, a relative permeability of 84, and a coercivity of Hc of 92 A / m.

[0086] Example 2

[0087] This embodiment describes a high-performance iron-based magnetostrictive alloy sheet, wherein the sheet has a thickness of 0.20 mm and a composition of (Fe... 0.8 Ga 0.16 Al 0.04 ) 99.75 B 0.2 Nd 0.05 .

[0088] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0089] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0090] S2. Raw material proportioning and weighing: According to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet, the raw materials for the pretreatment in S1 are weighed and proportioned. The proportioning needs to take into account the burning loss, which includes Ga burning loss, and the burning loss is 5%, to obtain the prepared raw materials. The prepared raw materials include Fe, Ga and Al with a purity greater than 99.9%, rare earth element Nd with a purity greater than 99.99%, and B is added in the form of Fe-B master alloy (B mass ratio 20%).

[0091] S3. Alloy Billet Preparation: The prepared raw material of S2 is used in a vacuum induction furnace. After evacuation, Ar is introduced as a protective gas, and the furnace is induction heated until completely melted. The mixture is then refined for 3 minutes until the composition is homogeneous. The billet is then poured into a directional solidification mold. After directional solidification, a billet with the desired shape is obtained. <100> Orientation and columnar crystal structure yield a uniformly composed alloy billet;

[0092] S4. Hot forging: The alloy billet with uniform composition of S3 is homogenized and annealed at 980℃ for 8 hours, and then hot forged into a slab. The hot forging temperature is 1030℃, the deformation per hot forging is controlled at 7%, and the total deformation is 60%, to obtain alloy forging material.

[0093] S5. Hot rolling + warm rolling + cold rolling: The S4 alloy forging is subjected to hot rolling + warm rolling + cold rolling. The initial rolling temperature of hot rolling is 1050℃, with 8 rolling passes, a reduction of 9% per pass, and a total reduction of 72%. The final rolling temperature is not lower than 830℃. After hot rolling, it is air-cooled to room temperature. The rolling temperature of warm rolling is 400℃, with 15 rolling passes, a reduction of 5% per pass, and a total reduction of 75%. After warm rolling, it is air-cooled to room temperature. After pickling, the warm-rolled plate is cold-rolled at room temperature with 25 rolling passes, a reduction of 2.5% per pass, and a total reduction of 62.5%, to obtain a 0.20mm thick iron-based magnetostrictive alloy sheet.

[0094] S6. Three-stage heating heat treatment + TbCu diffusion heat treatment: The three-stage heating heat treatment of the iron-based magnetostrictive alloy sheet after rolling of S5 needs to be carried out in an ammonia-argon-nitrogen mixed atmosphere (ammonia volume ratio of 12% and nitrogen volume ratio of 40%). First, the temperature is raised from room temperature to the initial recrystallization temperature of 850℃ at a heating rate of 8℃ / min and held for 15min. Then, the temperature is raised from the initial recrystallization temperature to the secondary recrystallization start temperature of 930℃ at a heating rate of 20℃ / min without holding. After that, the temperature is raised from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 1180℃ at a heating rate of 0.75℃ / min. The flowing atmosphere is changed to pure argon. After the heating is completed, the temperature is held for 4h. After the holding is completed, the temperature is air-cooled to room temperature.

[0095] Then, a TbCu diffusion heat treatment is performed to deposit a Tb layer with a thickness of approximately 20-30 micrometers. 0.5 Cu 0.5 The alloy rapid quenching strip is spread on both sides of the thin plate, heated to 1240℃ at a heating rate of 15℃ / min, held at that temperature for 3 hours, and then water quenched to cool to room temperature to obtain the finished iron-based magnetostrictive alloy thin plate.

[0096] The high-performance iron-based magnetostrictive alloy sheet prepared in this embodiment will have a strong Gaussian texture or cubic texture along the rolling direction. Nd is dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing a cluster of locally ordered structures.

[0097] The high-performance iron-based magnetostrictive (Fe) prepared in this embodiment 0.8 Ga 0.16 Al 0.04 ) 99.75 B 0.2 Nd0.05 The density of the finished alloy sheet is 7.81 g / cm³. 3 The hardness is 214HV, the tensile strength is 531MPa, and the elongation is 4.3%; Figure 2 As shown, under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 153 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 368 ppm; the Curie temperature is 658℃, the saturation magnetic induction intensity is 1.52 T, and the resistivity is 92 × 10⁻⁶. -8 It has a strength of Ω·cm, a relative permeability of 79, and a coercivity of Hc of 103 A / m.

[0098] Example 3

[0099] This embodiment describes a high-performance iron-based magnetostrictive alloy sheet, wherein the sheet has a thickness of 0.22 mm and a composition of (Fe... 0.8 Ga 0.17 ) 99.75 Mn 0.1 (TiC) 0.1 Ho 0.05 .

[0100] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0101] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0102] S2. Raw material proportioning and weighing: According to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet, the raw materials for the pretreatment in S1 are weighed and proportioned. The proportioning needs to take into account the burning loss, which includes Ga burning loss, and the burning loss is 5%, to obtain the prepared raw materials. The prepared raw materials include Fe, Ga, Mn and Ti with a purity greater than 99.9%, rare earth element Ho with a purity greater than 99.99%, and C is added in the form of Fe-C master alloy.

[0103] S3. Alloy Billet Preparation: The prepared raw material of S2 is used in a vacuum induction furnace. After evacuation, Ar is introduced as a protective gas, and the furnace is induction heated until completely melted. The mixture is then refined for 3 minutes until the composition is homogeneous. The billet is then poured into a directional solidification mold. After directional solidification, a billet with the desired shape is obtained. <100> Orientation and columnar crystal structure yield a uniformly composed alloy billet;

[0104] S4. Hot forging: The alloy billet with uniform composition of S3 is homogenized and annealed at 980℃ for 7 hours, and then hot forged into a slab. The hot forging temperature is 1020℃, the deformation per hot forging is controlled at 8%, and the total deformation is 60%, to obtain alloy forging material.

[0105] S5, Hot Rolling + Warm Rolling + Cold Rolling: The S4 alloy forging is subjected to hot rolling + warm rolling + cold rolling. The initial rolling temperature of hot rolling is 1100℃, with 8 rolling passes, a reduction of 8% per pass, and a total reduction of 64%. The final rolling temperature is not lower than 830℃. After hot rolling, it is air-cooled to room temperature. The rolling temperature of warm rolling is 420℃, with 15 rolling passes, a reduction of 5% per pass, and a total reduction of 75%. After warm rolling, it is air-cooled to room temperature. After pickling, the warm-rolled plate is cold-rolled at room temperature with 25 rolling passes, a reduction of 2% per pass, and a total reduction of 50%, to obtain a 0.22mm thick iron-based magnetostrictive alloy sheet.

[0106] S6. Three-stage heating heat treatment + TbCu diffusion heat treatment: The three-stage heating heat treatment of the iron-based magnetostrictive alloy sheet after rolling of S5 needs to be carried out in an ammonia-argon-nitrogen mixed atmosphere (ammonia volume ratio of 8% and nitrogen volume ratio of 35%). First, the temperature is raised from room temperature to the initial recrystallization temperature of 850℃ at a heating rate of 8℃ / min and held for 15min. Then, the temperature is raised from the initial recrystallization temperature to the secondary recrystallization start temperature of 920℃ at a heating rate of 20℃ / min without holding. After that, the temperature is raised from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 1160℃ at a heating rate of 0.70℃ / min. The flowing atmosphere is changed to pure argon. After the heating is completed, the temperature is held for 4h. After the holding is completed, the temperature is air-cooled to room temperature.

[0107] Then, a TbCu diffusion heat treatment is performed to deposit a Tb layer with a thickness of approximately 20-30 micrometers. 0.4 Cu 0.6 The alloy rapid quenching strip is spread on both sides of the thin plate, and the temperature is raised to 1220℃ at a heating rate of 13℃ / min. After holding at this temperature for 2 hours, it is quenched in salt water and cooled to room temperature to obtain the finished iron-based magnetostrictive alloy thin plate.

[0108] The high-performance iron-based magnetostrictive alloy sheet prepared in this embodiment will have a strong Gaussian texture or cubic texture along the rolling direction. Ho is dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing a cluster of locally ordered structures.

[0109] The high-performance iron-based magnetostrictive (Fe) prepared in this embodiment 0.83 Ga 0.17 ) 99.75 Mn 0.1 (TiC) 0.1 Ho0.05 The density of the finished alloy sheet is 7.85 g / cm³. 3 The hardness is 223HV, the tensile strength is 435MPa, and the elongation is 4.2%; Figure 3 As shown, under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 208 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 365 ppm; the Curie temperature is 661℃, the saturation magnetic induction intensity is 1.53 T, and the resistivity is 94 × 10⁻⁶. -8 Ω·cm, relative permeability 75, coercivity Hc 109 A / m.

[0110] Example 4

[0111] This embodiment describes a high-performance iron-based magnetostrictive alloy sheet, wherein the sheet has a thickness of 0.15 mm and a composition of (Fe... 0.79 Ga 0.16 Cr 0.05 ) 99.63 (ZrB) 0.3 Gd 0.07 .

[0112] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0113] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0114] S2. Raw material proportioning and weighing: Weigh the pretreatment raw materials for S1 according to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet. The proportioning needs to take into account the burning loss, which includes Ga burning loss, and the burning loss is 5%, to obtain the prepared raw materials. The prepared raw materials include Fe, Ga, Cr and Zr with a purity greater than 99.9%, rare earth element Gd with a purity greater than 99.99%, and B is added in the form of Fe-B master alloy (B mass ratio 20%).

[0115] S3. Alloy Billet Preparation: The prepared raw material of S2 is used in a vacuum induction furnace. After evacuation, Ar is introduced as a protective gas, and the furnace is induction heated until completely melted. The mixture is then refined for 3 minutes until the composition is homogeneous. The billet is then poured into a directional solidification mold. After directional solidification, a billet with the desired shape is obtained. <100> Orientation and columnar crystal structure yield a uniformly composed alloy billet;

[0116] S4. Hot forging: The alloy billet with uniform composition of S3 is homogenized and annealed at 990℃ for 8 hours, and then hot forged into a slab. The hot forging temperature is 1020℃, the deformation per hot forging is controlled at 6%, and the total deformation is 65%, to obtain alloy forging material.

[0117] S5, Hot Rolling + Warm Rolling + Cold Rolling: The S4 alloy forging is subjected to hot rolling + warm rolling + cold rolling. The initial rolling temperature of hot rolling is 1020℃, with 9 rolling passes, a reduction of 9% per pass, and a total reduction of 81%. The final rolling temperature is not lower than 830℃. After hot rolling, it is air-cooled to room temperature. The rolling temperature of warm rolling is 450℃, with 12 rolling passes, a reduction of 6% per pass, and a total reduction of 72%. After warm rolling, it is air-cooled to room temperature. After pickling, the warm-rolled plate is cold-rolled at room temperature with 28 rolling passes, a reduction of 3% per pass, and a total reduction of 84%, to obtain a 0.15mm thick iron-based magnetostrictive alloy sheet.

[0118] S6. Three-stage heating heat treatment + TbCu diffusion heat treatment: The three-stage heating heat treatment of the iron-based magnetostrictive alloy sheet after rolling of S5 needs to be carried out in an ammonia-argon-nitrogen mixed atmosphere (ammonia volume ratio of 10% and nitrogen volume ratio of 40%). First, the temperature is raised from room temperature to the initial recrystallization temperature of 820℃ at a heating rate of 8℃ / min and held for 15min. Then, the temperature is raised from the initial recrystallization temperature to the secondary recrystallization start temperature of 950℃ at a heating rate of 20℃ / min without holding. After that, the temperature is raised from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 1150℃ at a heating rate of 0.75℃ / min. The flowing atmosphere is changed to pure argon. After the heating is completed, the temperature is held for 4h. After the holding is completed, the temperature is air-cooled to room temperature.

[0119] Then, a TbCu diffusion heat treatment is performed to deposit a Tb layer with a thickness of approximately 20-30 micrometers. 0.5 Cu 0.5 The alloy rapid quenching strip is spread on both sides of the thin plate, and the temperature is raised to 1230℃ at a heating rate of 15℃ / min. After holding at this temperature for 3 hours, it is water quenched and cooled to room temperature to obtain the finished iron-based magnetostrictive alloy thin plate.

[0120] The high-performance iron-based magnetostrictive alloy sheet prepared in this embodiment will have a strong Gaussian texture or cubic texture along the rolling direction. Gd and Tb are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing a cluster of locally ordered structures.

[0121] The high-performance iron-based magnetostrictive (Fe) prepared in this embodiment 0.8 Ga 0.16 Cr 0.05 ) 99.63 (ZrB) 0.3Gd 0.07 The density of the finished alloy sheet is 7.79 g / cm³. 3 The hardness is 224 HV, the tensile strength is 511 MPa, and the elongation is 3.8%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 203 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 358 ppm. The Curie temperature is 654℃, the saturation magnetic induction is 1.59 T, and the resistivity is 83 × 10⁻⁶. -8 It has a strength of Ω·cm, a relative permeability of 86, and a coercivity of Hc of 105 A / m.

[0122] Example 5

[0123] This embodiment describes a high-performance iron-based magnetostrictive alloy sheet, wherein the thickness of the high-performance iron-based magnetostrictive alloy sheet is 0.18 mm, and the composition is (Fe 0.81 Ga 0.19 ) 99.35 (NbC) 0.1 B 0.5 Tb 0.05 .

[0124] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0125] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0126] S2. Raw material proportioning and weighing: According to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet, the raw materials for the pretreatment in S1 are weighed and proportioned. The proportioning needs to take into account the burning loss, which includes Ga burning loss, and the burning loss is 5%, to obtain the prepared raw materials. The prepared raw materials include Fe, Ga and Nb with a purity greater than 99.9%, rare earth element Tb with a purity greater than 99.99%, B is added in the form of Fe-B master alloy (B mass ratio 20%), and C is added in the form of Fe-C master alloy.

[0127] S3. Alloy Billet Preparation: The prepared raw material of S2 is used in a vacuum induction furnace. After evacuation, Ar is introduced as a protective gas, and the furnace is induction heated until completely melted. The mixture is then refined for 3 minutes until the composition is homogeneous. The billet is then poured into a directional solidification mold. After directional solidification, a billet with the desired shape is obtained. <100> Orientation and columnar crystal structure yield a uniformly composed alloy billet;

[0128] S4. Hot forging: The alloy billet with uniform composition of S3 is homogenized and annealed at 1000℃ for 8 hours, and then hot forged into a slab. The hot forging temperature is 1050℃, the deformation per hot forging is controlled at 8%, and the total deformation is 65%, to obtain alloy forging material.

[0129] S5, Hot Rolling + Warm Rolling + Cold Rolling: The S4 alloy forging is subjected to hot rolling + warm rolling + cold rolling. The initial rolling temperature of hot rolling is 1040℃, with 10 rolling passes, a reduction of 8% per pass, and a total reduction of 80%. The final rolling temperature is not lower than 830℃. After hot rolling, it is air-cooled to room temperature. The rolling temperature of warm rolling is 420℃, with 14 rolling passes, a reduction of 5% per pass, and a total reduction of 70%. After warm rolling, it is air-cooled to room temperature. After pickling, the warm-rolled plate is cold-rolled at room temperature with 25 rolling passes, a reduction of 3% per pass, and a total reduction of 75%, to obtain a 0.18mm thick iron-based magnetostrictive alloy sheet.

[0130] S6. Three-stage heating heat treatment + TbCu diffusion heat treatment: The three-stage heating heat treatment of the iron-based magnetostrictive alloy sheet after rolling of S5 needs to be carried out in an ammonia-argon-nitrogen mixed atmosphere (ammonia volume ratio of 12% and nitrogen volume ratio of 45%). First, the temperature is raised from room temperature to the initial recrystallization temperature of 840℃ at a heating rate of 8℃ / min and held for 14min. Then, the temperature is raised from the initial recrystallization temperature to the secondary recrystallization start temperature of 950℃ at a heating rate of 20℃ / min without holding. After that, the temperature is raised from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 1150℃ at a heating rate of 0.65℃ / min. The flowing atmosphere is changed to pure argon. After the heating is completed, the temperature is held for 4.5h. After the holding is completed, the temperature is air-cooled to room temperature.

[0131] Then, TbCu diffusion heat treatment was performed to expand the Dy layer to a thickness of approximately 20-30 micrometers. 0.5 Cu 0.5 The alloy rapid quenching strip is spread on both sides of the thin plate, heated to 1200℃ at a heating rate of 15℃ / min, held at that temperature for 3 hours, and then water quenched to cool to room temperature to obtain the finished iron-based magnetostrictive alloy thin plate.

[0132] The high-performance iron-based magnetostrictive alloy sheet prepared in this embodiment will have a strong Gaussian texture or cubic texture along the rolling direction. Tb and Dy are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing a cluster of locally ordered structures.

[0133] The high-performance iron-based magnetostrictive (Fe) prepared in this embodiment 0.81 Ga 0.19 ) 99.35 (NbC) 0.1 B 0.5Tb 0.05 The density of the finished alloy sheet is 7.74 g / cm³. 3 The hardness is 214 HV, the tensile strength is 562 MPa, and the elongation is 4.3%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 211 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 359 ppm. The Curie temperature is 642℃, the saturation magnetic induction is 1.61 T, and the resistivity is 94 × 10⁻⁶. -8 It has a strength of Ω·cm, a relative permeability of 83, and a coercivity of Hc of 116 A / m.

[0134] Example 6

[0135] This embodiment describes a high-performance iron-based magnetostrictive alloy sheet, wherein the sheet has a thickness of 0.08 mm and a composition of (Fe... 0.8 Ga 0.12 Al 0.08 ) 99.38 (TiC) 0.1 B 0.5 Y 0.02 .

[0136] A method for preparing a high-performance iron-based magnetostrictive alloy thin plate, comprising the following preparation steps:

[0137] S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials;

[0138] S2. Raw material proportioning and weighing: According to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet, the raw materials for the pretreatment in S1 are weighed and proportioned. The proportioning needs to take into account the burning loss, which includes Ga burning loss, and the burning loss is 5%, to obtain the prepared raw materials. The prepared raw materials include Fe, Ga, Al and Ti with a purity greater than 99.9%, element Y with a purity greater than 99.99%, B is added in the form of Fe-B master alloy (B mass ratio 20%), and C is added in the form of Fe-C master alloy.

[0139] S3. Alloy Billet Preparation: The prepared raw material of S2 is used in a vacuum induction furnace. After evacuation, Ar is introduced as a protective gas, and the furnace is induction heated until completely melted. The mixture is then refined for 3 minutes until the composition is homogeneous. The billet is then poured into a directional solidification mold. After directional solidification, a billet with the desired shape is obtained. <100> Orientation and columnar crystal structure yield a uniformly composed alloy billet;

[0140] S4. Hot forging: The alloy billet with uniform composition of S3 is homogenized and annealed at 990℃ for 8 hours, and then hot forged into a slab. The hot forging temperature is 1050℃, the deformation per hot forging is controlled at 8%, and the total deformation is 70%, to obtain alloy forging material.

[0141] S5, Hot Rolling + Warm Rolling + Cold Rolling: The S4 alloy forging is subjected to hot rolling + warm rolling + cold rolling. The initial rolling temperature of hot rolling is 1050℃, with 10 rolling passes, a reduction of 8.5% per pass, and a total reduction of 85%. The final rolling temperature is not lower than 830℃. After hot rolling, it is air-cooled to room temperature. The rolling temperature of warm rolling is 450℃, with 18 rolling passes, a reduction of 5% per pass, and a total reduction of 90%. After warm rolling, it is air-cooled to room temperature. After pickling, the warm-rolled plate is cold-rolled at room temperature with 30 rolling passes, a reduction of 2.5% per pass, and a total reduction of 75%, to obtain a 0.08mm thick iron-based magnetostrictive alloy sheet.

[0142] S6. Three-stage heating heat treatment + TbCu diffusion heat treatment: The three-stage heating heat treatment of the iron-based magnetostrictive alloy sheet after rolling of S5 needs to be carried out in an ammonia-argon-nitrogen mixed atmosphere (ammonia volume ratio of 18% and nitrogen volume ratio of 40%). First, the temperature is raised from room temperature to the initial recrystallization temperature of 850℃ at a heating rate of 8℃ / min and held for 10min. Then, the temperature is raised from the initial recrystallization temperature to the secondary recrystallization start temperature of 910℃ at a heating rate of 20℃ / min without holding. After that, the temperature is raised from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 1160℃ at a heating rate of 0.95℃ / min. The flowing atmosphere is changed to pure argon. After the heating is completed, the temperature is held for 4.5h. After the holding is completed, the temperature is air-cooled to room temperature.

[0143] Then, a TbCu diffusion heat treatment is performed to deposit a Tb layer with a thickness of approximately 20-30 micrometers. 0.4 Cu 0.6 The alloy rapid quenching strip is spread on both sides of the thin plate, heated to 1260℃ at a heating rate of 15℃ / min, held at that temperature for 3.5h, and then water quenched to cool to room temperature to obtain the finished iron-based magnetostrictive alloy thin plate.

[0144] The high-performance iron-based magnetostrictive alloy sheet prepared in this embodiment will have a strong Gaussian texture or cubic texture along the rolling direction. Y and Tb are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing a cluster of locally ordered structures.

[0145] The high-performance iron-based magnetostrictive (Fe) prepared in this embodiment 0.8 Ga 0.12 Al 0.08 ) 99.38 (TiC)0.1 B 0.5 Y 0.02 The density of the finished alloy sheet is 7.85 g / cm³. 3 The hardness is 222 HV, the tensile strength is 501 MPa, and the elongation is 4.4%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 183 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 354 ppm. The Curie temperature is 657℃, the saturation magnetic induction is 1.62 T, and the resistivity is 86 × 10⁻⁶. -8 It has a strength of Ω·cm, a relative permeability of 75, and a coercivity of Hc of 121 A / m.

[0146] The present invention proposes a high-performance iron-based magnetostrictive alloy thin plate and its preparation method, which solves the technical problems of insufficient texture control stability, low mechanical properties and magnetostrictive properties in existing magnetostrictive alloy thin plate technology.

[0147] This invention employs the principle of "organic inheritance" based on initial orientation, combined with the principle of inducing abnormal grain growth by using finely dispersed second-phase precipitation (carbide, nitride, carbonitride, or rare-earth-rich precipitates) and surface energy regulation. By controlling the heat treatment process (temperature, time, atmosphere, heating and cooling rates, diffusion heat treatment, and final cooling rate, etc.), a macroscopic structure with strong Gaussian or cubic texture and grain size reaching several centimeters is obtained, similar to a single-crystal structure, which is beneficial for improving magnetostrictive properties.

[0148] This invention is based on the principle of "nano-heterogeneous structure". After a thin plate has undergone three-stage heating heat treatment, it is subjected to (Tb / Dy)Cu diffusion heat treatment. The plate is heated to 1250-1350℃ and held for 2-4 hours, followed by water quenching or salt water quenching to room temperature. This forces one or more elements such as La, Ce, Pr, Nd, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr to dissolve in the alloy matrix. This induces locally ordered structures or structural clusters (B2-like or M-DO3 or L60 structures) in the disordered A2 structure of the matrix. Microscopically, this forms a microstructure feature of disordered matrix containing locally ordered structural clusters, which further improves the magnetostrictive properties of the alloy thin plate.

[0149] The high-performance iron-based magnetostrictive alloy thin sheet prepared by the method of this invention has a density of 7.52-7.91 g / cm³. 3The hardness is 213-242 HV, the tensile strength is 410-720 MPa, and the elongation is 2-5%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 150-230 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 350-390 ppm. The Curie temperature is >650℃, the saturation magnetic induction intensity is 1.44-1.68 T, and the resistivity is 83 × 10⁻⁶. -8 -96×10 -8 Ω·cm, relative permeability 72-109, coercivity Hc 89-126 A / m.

[0150] The high-performance iron-based magnetostrictive alloy sheet of the present invention has a thickness between 0.05-0.5 mm, low eddy current loss, and can be applied to different frequency requirements.

[0151] The material preparation process of this invention is not demanding, has low cost, and is conducive to widespread application.

[0152] In summary, compared with the magnetostrictive alloy sheet technology, the method of this invention prepares high-performance iron-based magnetostrictive alloy sheets with improved magnetostrictive properties through raw material pretreatment, raw material proportioning and weighing, alloy billet preparation, hot forging, hot rolling + warm rolling + cold rolling, and three-stage heating heat treatment + (Tb / Dy)Cu diffusion heat treatment. This method is simple in process, easy to operate, low in cost, and high in efficiency. The prepared products have low eddy current loss and are applicable to a wide range of frequencies, which is conducive to large-scale industrial production and application.

[0153] It should be understood that the term "and / or" in this article is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. A and B can be singular or plural. Additionally, the character " / " in this article generally indicates an "or" relationship between the preceding and following related objects, but it can also represent an "and / or" relationship. Please refer to the context for a more accurate understanding.

[0154] In this invention, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of a single item or a plurality of items. For example, at least one of a, b, or c can represent: a, b, c, ab, ac, bc, or abc, where a, b, and c can be a single item or multiple items.

[0155] It should be understood that, in various embodiments of the present invention, the order of the above-mentioned process numbers does not imply the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present invention.

[0156] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A high-performance iron-based magnetostrictive alloy sheet, characterized in that, The high-performance iron-based magnetostrictive alloy sheet has a thickness of 0.05-0.5 mm and a composition of (Fe). 1-x-z Ga x Al y Cr z ) 100-a-b M a N b , where x=0.1-0.3, y=0.0-0.1, z=0.0-0.05, a=0.01-1.0, b=0.01-0.5, M is one or more of B, Nb, C, Ti, V, Mn, N and S, and N is one or more of La, Ce, Pr, Nd, Sm, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr.

2. The high-performance iron-based magnetostrictive alloy sheet according to claim 1, characterized in that, The high-performance iron-based magnetostrictive alloy sheet will acquire a strong Gaussian texture or cubic texture along the rolling direction. One or more of the elements N, La, Ce, Pr, Nd, Tb, Dy, Gd, Ho, Er, Y, Cu and Zr are dissolved in the alloy matrix, inducing a locally ordered structure or B2-like or M-DO3 or L60 structure in the disordered A2 structure of the matrix, forming a microscopic structural feature of a disordered matrix containing clusters of locally ordered structures.

3. The high-performance iron-based magnetostrictive alloy sheet according to claim 1, characterized in that, The density of the high-performance iron-based magnetostrictive alloy sheet is 7.52-7.91 g / cm³. 3 The hardness is 213-242 HV, the tensile strength is 410-720 MPa, and the elongation is 2-5%. Under a magnetic field of 500 Oe and a prestress of 10 MPa, the saturation magnetostriction coefficient in the direction parallel to the magnetic field is 150-230 ppm, and the saturation magnetostriction coefficient of (3 / 2)λs is 350-390 ppm. The Curie temperature is >650℃, the saturation magnetic induction intensity is 1.44-1.68 T, and the resistivity is 83 × 10⁻⁶. -8 -96×10 -8 Ω·cm, relative permeability 72-109, coercivity Hc 89-126 A / m.

4. A method for preparing a high-performance iron-based magnetostrictive alloy thin plate according to claim 1, characterized in that, The preparation method of the high-performance iron-based magnetostrictive alloy thin plate includes the following preparation steps: S1. Raw material pretreatment: Select raw materials according to the composition of the high-performance iron-based magnetostrictive alloy sheet, clean the surface of the raw materials, remove oxide scale and keep them dry to obtain pretreated raw materials; S2. Weighing and proportioning of raw materials: Weigh and proportion the pre-treated raw materials according to the composition ratio of the high-performance iron-based magnetostrictive alloy sheet in S1. The proportion needs to take into account the burning loss to obtain the prepared raw materials. S3. Alloy billet preparation: The raw materials prepared in S2 are smelted in a vacuum induction furnace, magnetic levitation furnace or electric arc melting furnace to obtain an alloy billet with uniform composition. S4. Hot forging: After high-temperature homogenization annealing, the alloy billet with uniform composition of S3 is hot forged to obtain alloy forging material. S5, hot rolling + warm rolling + cold rolling: hot rolling + warm rolling + cold rolling of S4 alloy forgings to obtain iron-based magnetostrictive alloy thin plates; S6, Three-stage heating heat treatment + (Tb / Dy)Cu diffusion heat treatment: The iron-based magnetostrictive alloy sheet of S5 is subjected to three-stage heating heat treatment after rolling + (Tb / Dy)Cu diffusion heat treatment to obtain the finished iron-based magnetostrictive alloy sheet.

5. The method for preparing high-performance iron-based magnetostrictive alloy thin plates according to claim 4, characterized in that, The burn-off in S2 includes volatile elements such as Ga and Mn, with a burn-off rate of 2-5%.

6. The method for preparing high-performance iron-based magnetostrictive alloy thin plates according to claim 4, characterized in that, In S3 smelting, the vacuum level is first reduced to 10. -3 -10 -2 Argon gas at 400 Pa is then introduced and heated to melt the raw materials and form an alloy. After melting, the alloy is refined for 2-3 minutes to ensure the uniformity of the alloy composition. The refined alloy is then cast into alloy ingots or prepared into alloy rods through directional solidification.

7. The method for preparing high-performance iron-based magnetostrictive alloy thin plates according to claim 4, characterized in that, The high-temperature homogenization annealing temperature of S4 is 920-1050℃, and the holding time is 5-10h; the hot forging temperature is 900-1100℃, the deformation per heat is controlled at 5-10%, the total deformation is 50-70%, and the thickness of the alloy forging is 30-100mm.

8. The method for preparing high-performance iron-based magnetostrictive alloy thin plates according to claim 4, characterized in that, S5 steel consists of hot rolling, warm rolling, and cold rolling. The initial rolling temperature for hot rolling is 900-1250℃, with 5-10 rolling passes, a reduction of 3-10% per pass, and a total reduction of 50-95%. The final rolling temperature is not lower than 830℃, and the steel is air-cooled to room temperature after hot rolling. The rolling temperature for warm rolling is 300-500℃, with 10-20 rolling passes, a reduction of 2-5% per pass, and a total reduction of 50-95%. The steel is air-cooled to room temperature after warm rolling. After pickling, the warm-rolled steel is cold-rolled at room temperature with 15-30 rolling passes, a reduction of 1-3% per pass, and a total reduction of 50-90%. The thickness of the iron-based magnetostrictive alloy sheet is between 0.05-0.5mm.

9. The method for preparing high-performance iron-based magnetostrictive alloy thin plates according to claim 4, characterized in that, In S6, the heat treatment involves heating and holding the gas under a flowing atmosphere containing ammonia. The flowing atmosphere is argon or a mixture of nitrogen and argon, wherein the volume ratio of nitrogen in the mixture is less than 50%, and the volume ratio of ammonia in the flowing atmosphere is 5-20%.

10. The method for preparing high-performance iron-based magnetostrictive alloy thin plates according to claim 4, characterized in that, The three-stage heat treatment in S6 is as follows: from room temperature to the initial recrystallization temperature of 780-880℃, the heating rate is 5-10℃ / min, and the holding time is 5-15min; from the initial recrystallization temperature to the secondary recrystallization start temperature of 780-950℃, the heating rate is 20-40℃ / min, and the holding time is not maintained; from the secondary recrystallization start temperature to the secondary recrystallization end temperature of 900-1250℃, the heating rate is 0.01-3℃ / min, and the holding time is maintained for 2-10h after the heating is completed, and then the temperature is air-cooled to room temperature after the holding time is completed. The diffusion heat treatment of (Tb / Dy)Cu is as follows: heat to 1250-1350℃ at a heating rate of 5-20℃ / min, hold for 2-4 hours, and then cool to room temperature by water quenching or brine quenching.

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