CN111323079A - Method for detecting comprehensive performance of amorphous alloy material - Google Patents
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Abstract
The invention relates to the field of alloy material detection, and provides a method for detecting comprehensive performance of an amorphous alloy material, wherein in the step S1, master alloy materials with different components are prepared by adopting a method of combining alternating current arc melting and high-frequency induction; step S2, preparing the master alloy materials with different components into amorphous alloy thin strips with series sizes by adopting a single-roller rapid quenching method; step S3, annealing the amorphous alloy thin strip with series sizes by different temperatures and stresses; step S4, magnetic property detection is carried out on the amorphous alloy thin strip; step S5, detecting the microstructure and the mechanical property of the amorphous alloy thin strip; step S6, detecting multi-shape phase change and tensile stress of the amorphous alloy thin strip; and S7, comprehensively counting, analyzing and testing results, and outputting comprehensive performance indexes of the amorphous alloy material. The method has comprehensive indexes and is easy to analyze various properties of the amorphous alloy material.
Description
Technical Field
The invention relates to the field of alloy material detection, in particular to a method for detecting comprehensive performance of an amorphous alloy material.
Background
Amorphous alloy (Amorphous Alloys) is solidified by super-quenching, atoms are not in time of orderly arranging and crystallizing when the alloy is solidified, the obtained solid alloy is a long-range disordered structure, has a unique Amorphous structure with short-range order and long-range disorder, and does not have the defects of crystal boundary, dislocation, distortion and the like existing in crystalline alloy, so that the Amorphous alloy has the excellent characteristics of high strength, high hardness, high wear resistance, high magnetic conductivity, high resistivity, low coercive force, low iron core loss and the like, is a very good soft magnetic material, can reduce the no-load loss of a distribution transformer by 60-80 percent, and is widely applied to the fields of transformers, high-temperature materials, anticorrosive materials, medicine, aerospace, military and the like.
The amorphous alloy has excellent performance due to the special microstructure, but the performance is determined by the processing technology and the composition of the amorphous alloy material, CN107177805B discloses an iron-based sub-nano alloy with good production manufacturability and a preparation method thereof, and the component expression of the iron-based sub-nano alloy is FeaSibBcCudMeXfWherein M is at least one element of Ti, Zr and Hf, X is at least one element of C, Ge, V, Cr, Mn, Mo, W, Zn and Sn, subscripts a, b, C, d, e and f are atom percentage contents of each corresponding element respectively, and the following conditions are met: a is more than or equal to 75 and less than or equal to 86, b is more than or equal to 2 and less than or equal to 9, c is more than or equal to 10 and less than or equal to 20, 0<d≤3，0<e≤3，0≤f≤2，0.5<e/d is less than or equal to 2, and a + b + c + d + e + f is 100; the preparation method comprises the following steps: 1) preparing materials: weighing and proportioning the raw materials with the mass percentage purity of not less than 99% according to the component expression of the alloy; 2) preparing a master alloy ingot: adding the raw materials of each component prepared in the step 1) into an induction melting furnace or an electric arc melting furnace, uniformly melting the raw materials, and then cooling along with the furnace or injecting the raw materials into a mold to be cooled into a master batchGold ingots; 3) preparing a sub-nanometer alloy strip: remelting the mother alloy ingot prepared in the step 2), and spraying the remelted mother alloy steel liquid onto the surface of a rapidly rotating copper roller by using a single-roller melt rapid quenching method to prepare the iron-based sub-nano alloy quenched strip consisting of an amorphous alloy matrix, sub-nano crystal grains and ordered atomic clusters.
The comprehensive properties of the amorphous alloy material comprise soft magnetic properties, mechanical properties, chemical properties and the like, and the comprehensive properties of the amorphous alloy material restrict the selection and application fields of the material.
Disclosure of Invention
Because the amorphous alloy material can obtain the dual-phase nanocrystalline alloy by annealing heat treatment at a proper temperature, the microstructure of the amorphous alloy material is that nano-scale grains are uniformly distributed in an amorphous substrate, and before the amorphous alloy material is applied in a large scale, the toughness and the brittleness, the magnetic performance and the microstructure of the amorphous alloy material need to be detected. The nano-crystalline grain size, volume fraction and tensile stress annealing process have direct influence on the comprehensive performance of the amorphous alloy material, and a detection method aiming at the comprehensive performance of the amorphous alloy material is lacked at present.
In view of the above, the present invention is directed to a method for detecting the comprehensive performance of an amorphous alloy material, the method comprises,
step S1, preparing master alloy materials with different components by adopting a method of combining alternating current arc melting and high-frequency induction;
step S2, preparing the master alloy materials with different components into amorphous alloy thin strips with series sizes by adopting a single-roller rapid quenching method;
step S3, annealing the amorphous alloy thin strips with series sizes at different temperatures and stresses;
step S4, magnetic property detection is carried out on the amorphous alloy thin strip;
step S5, detecting the microstructure and the mechanical property of the amorphous alloy thin strip;
step S6, detecting the multi-shape phase change and the tensile stress of the amorphous alloy thin strip;
and step S7, comprehensively counting, analyzing and testing results, and outputting comprehensive performance indexes of the amorphous alloy material.
Preferably, step S4 includes,
step S41, measuring a magnetic hysteresis loop of the amorphous alloy thin strip sample by using a vibration sample magnetometer, and analyzing magnetic performance parameters;
step S42, measuring the giant magneto-impedance effect curve of the series of samples by using an impedance meter;
and step S43, winding different amorphous alloy thin strip samples into transformers, and measuring the core loss under different frequencies and magnetization states.
Preferably, step S5 includes,
step S51, testing the XRD spectrum of the amorphous alloy thin strip sample by using a conventional XRD and projection XRD technology, and analyzing the microstructure of the sample;
step S52, analyzing the surface and fracture mesostructure of the amorphous alloy thin strip sample by AFM, SEM or TEM technology;
step S53, observing the surface and fracture magnetic domain structure of the amorphous alloy thin strip sample by using MFM technology;
and step S54, testing the mechanical property of the amorphous alloy thin strip sample.
Preferably, step S6 includes,
step S61, dynamically characterizing the structure of the nano system in situ by using a synchrotron radiation technology, and detecting a structural factor S (Q) and a radial distribution function g (r, r') of the polymorphic phase change process and the tensile stress low annealing process of the amorphous alloy thin strip;
step S62, fitting high-precision synchrotron radiation XRD data and EXAFS data by applying an inverse Monte Carlo (RMC) simulation method, and establishing an amorphous alloy thin strip polymorphic phase change structure model;
and step S63, calculating the polymorphic phase change mapping relation of the amorphous alloy thin strip induced by the tensile stress low-temperature annealing by using the model.
Preferably, the master alloy materials of different compositions in step S1 include fecunbbib, fesibbpcu, FeCuB, FeCuSiB, fecunbbib, FePC, FeSiB.
Preferably, the series of dimensions in step S2 includes the width and thickness of the amorphous alloy thin strip.
Preferably, in the step S3, the annealing treatment includes different annealing temperatures, annealing times, and annealing tensile stresses, and the annealing tensile stresses are 100-700 MPa.
Preferably, the annealing temperature is 300-.
Preferably, the thin amorphous alloy strip comprises Fe73.5Cu1Nb3Si13.5B9Amorphous alloy thin strip and different components Fe83.3-84.3Si4B8P3-4Cu0.7Amorphous alloy ribbon, FeCuB, FeCuSiB and FeCuNbSiB amorphous alloy ribbons with different components and high iron content, and FePC and FeSiB amorphous alloy ribbons with different components.
Preferably, in step S7, the performance index V of the amorphous alloy material is weighted according to A, B, C, where α, β, and γ are weights, and α + β + γ is 1;
wherein, the magnetic property of the amorphous alloy ribbon is detected by S4, and the magnetic property is A, xiThe magnetic performance indexes are the ith magnetic performance indexes, and the magnetic performance indexes comprise saturation magnetization intensity, magnetic conductivity and iron core loss;
A＝[x1x2x3… xn-1xn]
wherein, the microstructure and the mechanical property of the S5 pair amorphous alloy thin strip are B and yjThe j mechanical property indexes comprise strength, hardness, microstructure image, toughness and wear resistance;
B＝[y1y2y3… ym-1ym]
wherein, the performance, w, of the annealing phase change index parameter of the amorphous alloy thin strip reflected by S6kThe obtained h phase change index parameters comprise a structural factor S (Q), a radial distribution function g (r, r'), XRD data and EXAFS data;
C＝[w1w2w3… wh-1Wh]。
compared with the prior art, the method for detecting the comprehensive performance of the amorphous alloy material evaluates the performance of the amorphous alloy material from comprehensive angles of magnetic performance, mechanical performance, microstructure, polymorphic phase change and tensile stress, so that the comprehensive performance index of the amorphous alloy material is output, the index is comprehensive, and various performances of the amorphous alloy material are easy to analyze.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic general flow chart of an embodiment of a method for detecting comprehensive properties of an amorphous alloy material according to the present invention;
FIG. 2 is a flowchart in step S4 of one embodiment of a method for detecting comprehensive properties of an amorphous alloy material in FIG. 1;
FIG. 3 is a flowchart in step S5 of one embodiment of a method for detecting comprehensive properties of an amorphous alloy material in FIG. 1;
FIG. 4 is a flowchart in step S6 of one embodiment of a method for detecting comprehensive properties of an amorphous alloy material in FIG. 1;
FIG. 5 shows the preparation of Fe at different roll speeds82.65Si4B12Cu1.35And Fe82.65-xCu1.35(Si4B12)1+x/16XRD spectrogram of alloy quenched sample.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In order to solve the problems pointed out in the background art, before the amorphous alloy material is applied in a large scale, the toughness and the brittleness, the magnetic performance and the microstructure of the amorphous alloy material must be detected, and a method for detecting the comprehensive performance of the amorphous alloy material is lacked. The invention provides a method for detecting the comprehensive performance of an amorphous alloy material, which comprises the following steps of, as shown in figures 1-4,
step S1, preparing master alloy materials with different components by adopting a method of combining alternating current arc melting and high-frequency induction;
step S2, preparing the master alloy materials with different components into amorphous alloy thin strips with series sizes by adopting a single-roller rapid quenching method;
step S3, annealing the amorphous alloy thin strips with series sizes at different temperatures and stresses;
step S4, magnetic property detection is carried out on the amorphous alloy thin strip;
step S5, detecting the microstructure and the mechanical property of the amorphous alloy thin strip;
step S6, detecting the multi-shape phase change and the tensile stress of the amorphous alloy thin strip;
and step S7, comprehensively counting, analyzing and testing results, and outputting comprehensive performance indexes of the amorphous alloy material.
In step S1, the ac arc melting is to melt the iron material and overheat the molten iron by using heat generated by the arc generated between the graphite electrode and the iron material; the high frequency induction is to heat and melt the iron material by using heat generated by high frequency current induction.
In step S2, the single-roll rapid quenching method, also called melt-cooled roll-spinning method, is a method for producing an amorphous alloy ribbon.
In order to measure the magnetic properties of the amorphous alloy ribbon, including at least the saturation magnetization, permeability and core loss indexes, in a preferred aspect of the present invention, step S4 includes,
step S41, measuring a magnetic hysteresis loop of the amorphous alloy thin strip sample by using a vibration sample magnetometer, and analyzing magnetic performance parameters;
step S42, measuring the giant magneto-impedance effect curve of the series of samples by using an impedance meter;
and step S43, winding different amorphous alloy thin strip samples into transformers, and measuring the core loss under different frequencies and magnetization states.
Wherein, the vibrating sample Magnetometer in the step S41 comprises a Lake Shore vibrating sample Magnetometer VSM, vibrating sample Magnetometer 7407 or VSM 8604 or VSM8607, and generates a magnetization field with Hmax of ± 21000Oe, and the magnetic field control rate is 5000-; in step S32, the impedance meter includes an HP4294A type impedance meter.
In order to better measure the microstructure and mechanical properties of the amorphous alloy material, in a preferred aspect of the present invention, step S5 includes,
step S51, testing the XRD spectrum of the amorphous alloy thin strip sample by using a conventional XRD and projection XRD technology, and analyzing the microstructure of the sample;
step S52, analyzing the surface and fracture mesostructure of the amorphous alloy thin strip sample by AFM, SEM or TEM technology;
step S53, observing the surface and fracture magnetic domain structure of the amorphous alloy thin strip sample by using MFM technology;
and step S54, testing the mechanical property of the amorphous alloy thin strip sample.
In step S51, the synchrotron radiation XRD, X-ray Diffraction can measure the average information of the atomic structure from short to middle range, the electronic state information of the atoms with different components, the kind and number of the average neighboring atoms with the atoms with different components as the center, and the distance from the center atom in the amorphous alloy, as shown in FIG. 5, the embodiment Fe of the present invention82.65Si4B12Cu1.35And Fe82.65-xCu1.35(Si4B12)1+x/16XRD spectrum of the alloy.
In step S52, the surface and the fracture mesostructure of the series of samples are analyzed by an atomic force microscope AFM, a high resolution scanning electron microscope SEM or a transmission electron microscope TEM, and in step S53, the surface and the fracture magnetic domain structure of the series of samples are observed by a magnetic probe MFM technique.
In step S54, the mechanical properties include strength, hardness, toughness, and wear resistance.
In order to measure the polymorphic phase transformation structure of the amorphous alloy ribbon and further evaluate the external properties of the amorphous alloy, in a preferred aspect of the present invention, step S6 includes,
step S61, dynamically characterizing the structure of the nano system in situ by using a synchrotron radiation technology, and detecting a structural factor S (Q) and a radial distribution function g (r, r') of the polymorphic phase change process and the tensile stress low annealing process of the amorphous alloy thin strip;
step S62, fitting high-precision synchrotron radiation XRD data and EXAFS data by applying an inverse Monte Carlo (RMC) simulation method, and establishing an amorphous alloy thin strip polymorphic phase change structure model;
and step S63, calculating the polymorphic phase change mapping relation of the amorphous alloy thin strip induced by the tensile stress low-temperature annealing by using the model.
The EXAFS, Extended X-ray Absorption film Structure data refers to an expanded X-ray Absorption Fine Structure, and is based on scattering of photoelectrons emitted from central Absorption atoms by neighboring atoms, and can reflect the structural state of short-range order around the Absorption atoms in a substance.
In a preferred aspect of the present invention, the master alloy materials of different compositions in step S1 include fecunbbib, FeSiBPCu, FeCuB, FeCuSiB, fecunbbib, FePC, FeSiB.
In order to measure the properties of different series of amorphous alloy thin strips, in a preferred case of the present invention, the series of dimensions in step S2 includes the width and thickness of the amorphous alloy thin strip. More preferably, the amorphous alloy thin strip has a width of 100mm to 200mm and a thickness of 20 μm to 40 μm. In a more preferred aspect of the invention, the series of dimensions includes at least,
| thickness μm | 20 | 20 | 20 | 30 | 30 | 30 | 40 | 40 | 40 |
| Width mm | 100 | 160 | 200 | 100 | 160 | 200 | 100 | 160 | 200 |
Measuring the comprehensive properties of the amorphous alloy ribbon under the annealing processes with different annealing tensile stresses, annealing temperatures and annealing times, wherein in the preferred case of the invention, in the step S3, the annealing treatment comprises different annealing temperatures, annealing times and annealing tensile stresses, and the annealing tensile stress is 100-700 MPa. In a more preferred aspect of the invention, the annealing tensile stress varies by a value at least including,
| tensile stress MPa | 100 | 200 | 300 | 400 | 500 | 600 | 700 |
In order to measure the comprehensive properties of the amorphous alloy ribbon at different annealing temperatures, in the preferred case of the invention, the annealing temperature is 300-450 ℃, and in the more preferred case of the invention, the different values of the annealing temperature at least comprise 300 ℃, 350 ℃, 400 ℃ and 450 ℃.
In order to measure the comprehensive performance of the amorphous alloy thin strip under different annealing times, the different values of the annealing time at least comprise 1h, 1.5h, 2h, 2.5h, 3h, 4h and 6 h.
In order to test amorphous alloy thin strips with different compositions, in a preferred case of the invention, the amorphous alloy thin strips comprise Fe73.5Cu1Nb3Si13.5B9Amorphous alloy thin strip and different components Fe83.3-84.3Si4B8P3-4Cu0.7Amorphous alloy ribbon, FeCuB, FeCuSiB and FeCuNbSiB amorphous alloy ribbons with different components and high iron content, and FePC and FeSiB amorphous alloy ribbons with different components.
Detecting the magnetic property of the amorphous alloy thin strip by S4, wherein the magnetic property is A, xiThe magnetic performance indexes include saturation magnetization, magnetic conductivity and iron core loss.
A＝[x1x2x3… xn-1xn]
The microstructure and the mechanical property of the S5 pair amorphous alloy thin strip are B and yjThe j mechanical property indexes include strength, hardness, microstructure image, toughness and wear resistance.
B＝[y1y2y3… ym-1ym]
Performance, w, reflected by the annealing phase change index parameter of S6 to the amorphous alloy thin stripkThe h phase change index parameters obtained for the kth phase change index parameter include a structure factor s (q), a radial distribution function g (r, r'), XRD data, and EXAFS data.
C＝[W1w2w3… wh-1wh]
Before the amorphous alloy ribbon is applied, in step S7, the comprehensive performance index V of the amorphous alloy material is evaluated, and A, B, C performance indexes are weighted, so as to select a more suitable amorphous alloy ribbon, where α, β, and γ are weights, α + β + γ is 1, and the value is determined by the weight of the application field of the amorphous alloy ribbon.
In a more preferred aspect of the present invention, for example, in the application of transformer, it is preferable to select an amorphous alloy ribbon with good magnetic property, and α is the largest, and β and γ are considered in turn, and the value is α > β > γ.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for detecting the comprehensive performance of an amorphous alloy material is characterized by comprising the following steps of,
step S1, preparing master alloy materials with different components by adopting a method of combining alternating current arc melting and high-frequency induction;
step S2, preparing the master alloy materials with different components into amorphous alloy thin strips with series sizes by adopting a single-roller rapid quenching method;
step S3, annealing the amorphous alloy thin strips with series sizes at different temperatures and stresses;
step S4, magnetic property detection is carried out on the amorphous alloy thin strip;
step S5, detecting the microstructure and the mechanical property of the amorphous alloy thin strip;
step S6, detecting the multi-shape phase change and the tensile stress of the amorphous alloy thin strip;
and step S7, comprehensively counting, analyzing and testing results, and outputting comprehensive performance indexes of the amorphous alloy material.
2. The method for detecting the comprehensive performance of the amorphous alloy material as recited in claim 1, wherein the step S4 includes,
step S41, measuring a magnetic hysteresis loop of the amorphous alloy thin strip sample by using a vibration sample magnetometer, and analyzing magnetic performance parameters;
step S42, measuring the giant magneto-impedance effect curve of the series of samples by using an impedance meter;
and step S43, winding different amorphous alloy thin strip samples into transformers, and measuring the core loss under different frequencies and magnetization states.
3. The method for detecting the comprehensive performance of the amorphous alloy material as recited in claim 1, wherein the step S5 includes,
step S51, testing the XRD spectrum of the amorphous alloy thin strip sample by using a conventional XRD and projection XRD technology, and analyzing the microstructure of the sample;
step S52, analyzing the surface and fracture mesostructure of the amorphous alloy thin strip sample by AFM, SEM or TEM technology;
step S53, observing the surface and fracture magnetic domain structure of the amorphous alloy thin strip sample by using MFM technology;
and step S54, testing the mechanical property of the amorphous alloy thin strip sample.
4. The method for detecting the comprehensive performance of the amorphous alloy material as recited in claim 1, wherein the step S6 includes,
step S61, dynamically characterizing the structure of the nano system in situ by using a synchrotron radiation technology, and detecting a structural factor S (Q) and a radial distribution function g (r, r') of the polymorphic phase change process and the tensile stress low annealing process of the amorphous alloy thin strip;
step S62, fitting high-precision synchrotron radiation XRD data and EXAFS data by applying an inverse Monte Carlo (RMC) simulation method, and establishing an amorphous alloy thin strip polymorphic phase change structure model;
and step S63, calculating the polymorphic phase change mapping relation of the amorphous alloy thin strip induced by the tensile stress low-temperature annealing by using the model.
5. The method for detecting the comprehensive properties of the amorphous alloy material as claimed in claim 1, wherein the master alloy materials with different compositions in step S1 include fecunbbsb, fesibbpcu, FeCuB, FeCuSiB, fecunbbib, FePC, FeSiB.
6. The method as claimed in claim 1, wherein the series of dimensions in step S2 includes the width and thickness of the thin amorphous alloy strip.
7. The method as claimed in claim 1, wherein in step S3, the annealing treatment includes different annealing temperatures, annealing times, and annealing tensile stresses, and the annealing tensile stresses are 100-700 MPa.
8. The method as claimed in claim 7, wherein the annealing temperature is 300-450 ℃.
9. The method for detecting the comprehensive performance of the amorphous alloy material according to any one of claims 1 to 8, wherein the method is characterized in thatWherein the thin amorphous alloy strip comprises Fe73.5Cu1Nb3Si13.5B9Amorphous alloy thin strip and different components Fe83.3-84.3Si4B8P3-4Cu0.7Amorphous alloy ribbon, FeCuB, FeCuSiB and FeCuNbSiB amorphous alloy ribbons with different components and high iron content, and FePC and FeSiB amorphous alloy ribbons with different components.
10. The method as claimed in any of claims 1 to 8, wherein in step S7, the overall performance index V of the amorphous alloy material is weighted for each performance index A, B, C, where α, β, γ are weights, α + β + γ ═ 1;
wherein, the magnetic property of the amorphous alloy ribbon is detected by S4, and the magnetic property is A, xiThe magnetic performance indexes are the ith magnetic performance indexes, and the magnetic performance indexes comprise saturation magnetization intensity, magnetic conductivity and iron core loss;
A＝[x1x2x3… xn-1xn]
wherein, the microstructure and the mechanical property of the S5 pair amorphous alloy thin strip are B and yjThe j mechanical property indexes comprise strength, hardness, microstructure image, toughness and wear resistance;
B＝[y1y2y3… ym-1ym]
wherein, the performance, w, of the annealing phase change index parameter of the amorphous alloy thin strip reflected by S6kThe obtained h phase change index parameters comprise a structural factor S (Q), a radial distribution function g (r, r'), XRD data and EXAFS data;
C＝[w1w2w3… wh-1wh]。
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