CN115433812A - Method for improving tensile plasticity of toughened iron-based amorphous magnetically soft alloy strip - Google Patents
Method for improving tensile plasticity of toughened iron-based amorphous magnetically soft alloy strip Download PDFInfo
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
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- 230000001351 cycling effect Effects 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
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Classifications
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
- C21D1/44—Methods of heating in heat-treatment baths
- C21D1/50—Oil baths
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/04—Hardening by cooling below 0 degrees Celsius
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
Abstract
The invention discloses a method for improving the tensile plasticity of a toughened iron-based amorphous magnetically soft alloy strip, which comprises the following steps of carrying out cold-hot alternate circulation treatment on the prepared iron-based amorphous magnetically soft alloy strip; the temperature of the heat treatment is 0.4T g ‑0.6T g . The method of the invention ensures that the iron-based amorphous alloy keeps excellent soft magnetic performance, the high-temperature tensile plasticity is improved to more than 5 percent, and the annealing brittleness problem is effectively improved. The invention has the characteristics of simple process, convenient operation and strong flexibility and applicability, and can greatly expand the application of the iron-based amorphous alloy as a soft magnetic material.
Description
Technical Field
The invention relates to a method for amorphous post-treatment, in particular to a method for improving the tensile plasticity of a toughened iron-based amorphous magnetically soft alloy strip.
Background
The iron-based amorphous alloy is a novel green energy-saving material, has excellent soft magnetic properties such as high saturation magnetic induction intensity, low loss and high initial permeability, can replace traditional soft magnetic materials such as silicon steel, ferrite and permalloy, greatly reduces the energy consumption of power electronic equipment, and is widely applied to the fields of smart power grids, new-generation information technologies, rail transit, new energy automobiles and the like. However, iron-based amorphous soft magnetic alloys have a fatal weakness that they generally lack macroscopic plastic deformation capability and have negligible tensile plasticity [ Int Mater Rev 2013 (58): 131-166]. In addition, the best soft magnetic properties of Fe-based amorphous Alloys can be obtained only after stress relief annealing treatment, usually at higher temperature, which accelerates the relaxation process, causes the alloy to be sharply embrittled, and severely restricts the processability of Fe-based amorphous strips when being cut and wound into iron cores and the stability during subsequent use [ J Alloys Comp 2018 (657): 237-245]. Therefore, the method has important application value for improving the toughness and the plasticity of the iron-based amorphous soft magnetic alloy.
In the aspect of improving the toughness and plasticity of the iron-based amorphous soft magnetic alloy strip, researchers develop a great deal of exploratory work, and the main method comprises component exploration [ CN104131243A; CN109778082A and high temperature rapid annealing technique [ JMagn Magn Mater 2021 (523) 167583]. By increasing the Fe content or adding elements such as Ni and Mo with high Poisson ratio, the ductile-brittle transition temperature of the Fe-based amorphous magnetically soft alloy strip can be effectively increased, and the annealing brittleness can be improved. However, the component regulation and control method is difficult to ensure that the excellent soft magnetic performance of the alloy is kept unchanged, and meanwhile, a large number of repeated tests are often needed, which is accompanied by great consumption of manpower and material resources. The high-temperature rapid annealing technology has specific requirements on heating equipment, strip width and alloy oxidation resistance, and is difficult to meet all iron-based amorphous soft magnetic alloy systems.
As described above, although some studies have been conducted on improvement of plasticity of the iron-based amorphous soft magnetic alloy, the current method cannot satisfy improvement of plasticity of a large-scale sample. Therefore, it is necessary to further develop a method for regulating and controlling the energy state of the cold-hot cycle, and the toughness and plasticity of the iron-based amorphous alloy are improved on the premise of not reducing the soft magnetic performance by simple post-treatment on the basis of the original system.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a method for improving the tensile plasticity of a toughened iron-based amorphous magnetically soft alloy strip, which can reduce annealing brittleness and does not deteriorate good soft magnetic performance of the strip.
The technical scheme is as follows: the method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip comprises the following steps of carrying out cold-hot alternate circulating treatment on the prepared iron-based amorphous magnetically soft alloy strip; the temperature of the heat treatment is 0.4T g -0.6T g 。
The method comprises the following steps of placing an iron-based amorphous soft magnetic alloy strip in a hollow stainless steel ball, leading the steel ball out of a traction rope, and then carrying out cold-hot alternating circulation treatment.
Wherein the cold treatment process comprises the following steps: and putting the iron-based amorphous soft magnetic alloy strip in liquid nitrogen. The time for single soaking in liquid nitrogen is 30s-3min. The heat treatment process comprises the following steps: the iron-based amorphous soft magnetic alloy strip was placed in an oil bath.
Wherein the oil used for the oil bath is polydimethylsiloxane, and the oil bath temperature of between room temperature and 570K can be obtained. The time for single soaking in the oil bath pan is 30s-3min. According to the composition characteristics and the processing conditions of different iron-based amorphous alloys, different oil bath temperatures are selected, and the effective oil bath temperature range capable of realizing plasticity improvement is 0.4Tg-0.6Tg. T is a unit of g The glass transition temperature of the amorphous alloy.
Wherein, the number of the cold and hot alternate circulation is 10-30. The interval time of the cold and hot alternate circulation is 30s-3min.
Wherein the chemical molecular formula of the iron-based amorphous soft magnetic alloy strip is Fe in terms of atomic mole percentage x Co y B 19.2 Si 4.8 Nb 4 Cu z ，36≤x≤72，0≤y≤36，0≤z≤0.5，x+y+z＝72。
The invention principle is as follows: the intrinsic structure of the amorphous alloy has nonuniformity, so that the thermal expansion coefficients of different regions are inconsistent, and when the amorphous alloy is placed in liquid nitrogen and high temperature, the contraction and expansion coefficients of different regions are obviously different, so that local atom rearrangement is brought, the microstructure change is caused, and the nonuniform structure of the alloy is increased.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: (1) Through circulation in liquid nitrogen and hot oil, the tensile plasticity of the iron-based amorphous alloy is improved, the annealing brittleness is reduced, and the good soft magnetic performance of the iron-based amorphous alloy is not deteriorated. (2) The tensile plasticity of the iron-based amorphous alloy can be remarkably improved, the excellent soft magnetic property of the iron-based amorphous alloy is kept, and the application of the iron-based amorphous alloy as a soft magnetic material is greatly expanded. And (3) the process is simple, convenient to operate and flexible and high in applicability.
Drawings
FIG. 1 is a schematic diagram of an experimental procedure;
FIG. 2 shows [ (Fe) before and after cycles 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 X-ray diffraction pattern of the amorphous alloy;
FIG. 3 is the equation of { [ (Fe) before and after cycle 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 } 99.9 Cu 0.1 B-H curve of amorphous alloy;
FIG. 4 shows [ (Fe) before and after cycles 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The tensile stress-strain curve of the amorphous alloy strip at 693K;
FIG. 5 shows [ (Fe) before and after cycles 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The tensile stress-strain curve of the amorphous alloy strip at 643K;
FIG. 6 shows [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 Annealing the amorphous alloy strip for different time and then performing cold-hot circulating bending plasticity;
FIG. 7 shows [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 Straightening of amorphous alloy strip by cold-hot circulation after annealing at different timesHard to do.
Detailed Description
The present invention is described in further detail below.
Example 1
The molecular formula of the Fe-based amorphous alloy prepared in this example is [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The preparation process comprises the following steps:
And 2, distributing the weighed raw materials in a water-cooled copper mold crucible of the vacuum arc melting furnace in sequence according to the sequence of the melting points of the elements from low to high. Before smelting, the furnace chamber is vacuumized to 5 x 10 -3 Pa, and then filling argon to 0.7 atmosphere. During smelting, firstly smelting a titanium ingot in a furnace for 180 seconds to remove residual oxygen in a furnace cavity; when the target alloy is melted, the alloy is kept for 180 seconds after being completely melted. In order to obtain alloy ingots with uniform components, all samples are repeatedly smelted for 5 times, and the samples are turned over after each smelting.
And 3, removing surface impurities from the master alloy ingot obtained in the step 2, cleaning the master alloy ingot, crushing the master alloy ingot into small alloy ingots, and then carrying out spray casting on the master alloy ingots into bars with the diameter of 3mm in a vacuum spray casting furnace.
And 4, circularly processing the prepared bar, wherein the circulating parameters are set as follows: oil temperature 513K, cycle interval time of 3 minutes, cycle number of 10.
The specific preparation process is shown in figure 1.
Comparative example 1
The preparation molecular formula is [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The iron-based amorphous alloy.
The preparation is as described in example 1, except that no cold-hot cycles are carried out.
The samples of comparative example 1 and example 1 were ultrasonically cleanedAnd carrying out an X-ray diffraction test after blow-drying. The detailed test parameters are: the scanning step length is 0.02 degree/second, the scanning speed is 4 degrees/minute, and the scanning angle 2 theta range is 20 degrees-90 degrees. In FIG. 2, [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 X-ray diffraction patterns of the amorphous alloys comparative example 1 and example 1. It can be seen that [ (Fe) prepared in comparative example 1 and example 1 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The amorphous alloy curve shows two diffraction peaks which are widely dispersed without any sharp crystallization peak, which indicates that the alloy rod keeps an amorphous structure.
Example 2
The molecular formula of the iron-based amorphous alloy prepared by the embodiment is { [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 } 99.9 Cu 0.1 The preparation process comprises the following steps:
And 2, distributing the weighed raw materials in a water-cooled copper mold crucible of the vacuum arc melting furnace in sequence from low element melting point to high element melting point. Before smelting, the furnace chamber is vacuumized to 5 x 10 -3 Pa, and then filling argon to 0.7 atmosphere. During smelting, firstly smelting a titanium ingot in a furnace for 180 seconds to remove residual oxygen in a furnace cavity; when the target alloy is melted, the alloy is kept for 180 seconds after being completely melted. In order to obtain alloy ingots with uniform components, all samples are repeatedly smelted for 5 times, and the samples are turned over after each smelting.
And 3, preparing the master alloy ingot into a strip with the width of 1.2mm and the thickness of 0.22 mu m in a vacuum strip-casting furnace.
And 4, annealing the prepared strip at 755K for 20 minutes, and performing circulating treatment after annealing. The cycle parameters are set as: oil temperature 393K, cycle interval 30 seconds, cycle number 30 times.
Comparative example 2
The chemical formula of the preparation is { [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 } 99.9 Cu 0.1 The iron-based amorphous alloy.
The preparation is as described in example 2, with the difference that no cold-hot cycles are carried out after annealing.
The coercive force and saturation magnetic induction of the samples of comparative example 2 and example 2 were measured using a B-H meter and a vibrating sample magnetometer. FIG. 3 depicts before and after cycling { [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 } 99.9 Cu 0.1 Amorphous alloy B-H curve. It can be seen that { [ (Fe) prepared in comparative example 2 and example 2 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 } 99.9 Cu 0.1 The coercive force and the saturation magnetic induction of the amorphous strip are kept unchanged, which shows that the method of the invention does not damage the excellent soft magnetic performance of the Fe-based amorphous alloy.
Example 3
And 2, distributing the weighed raw materials in a water-cooled copper mold crucible of the vacuum arc melting furnace in sequence from low element melting point to high element melting point. Before smelting, the furnace chamber is vacuumized to 5 x 10 -3 Pa, and then filling argon to 0.7 atmosphere. During smelting, firstly smelting a titanium ingot in a furnace for 180 seconds to remove residual oxygen in a furnace cavity; when the target alloy was melted, the alloy was kept for 180 seconds after being completely melted. In order to obtain alloy ingots with uniform components, all samples are repeatedly smelted for 5 times, and the samples are turned over after each smelting.
And 3, preparing the master alloy ingot into a strip with the width of 0.56mm and the thickness of 0.17 mu m in a vacuum strip-casting furnace.
And 4, cutting partial strips and performing cyclic treatment on the strips. The cycle parameters are set as: oil temperature 563K, cycle interval time 1 minute, cycle number 15.
Comparative example 3
The chemical formula of the preparation is [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The iron-based amorphous alloy.
The preparation is as described in example 3, with the difference that no cooling-heating cycles are carried out.
The tensile properties at 643K were measured using a dynamic mechanical analyzer. FIG. 4 shows [ (Fe) prepared in comparative example 3 and example 3 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 Amorphous alloy tensile stress-strain curve. It can be seen that the tensile plasticity of the amorphous ribbon before cycling was 3% and that of the ribbon after cycling increased to 5.1%. Therefore, the method can improve the high-temperature tensile plasticity of the iron-based amorphous alloy.
Example 4
And 2, distributing the weighed raw materials in a water-cooled copper mold crucible of the vacuum arc melting furnace in sequence according to the sequence of the melting points of the elements from low to high. Before smelting, the furnace chamber is vacuumized to 5 x 10 -3 Pa, and then filling argon to 0.7 atmosphere. During smelting, firstly smelting a titanium ingot in a furnace for 180 seconds to remove residual oxygen in a furnace cavity; when the target alloy is melted, the alloy is kept for 180 seconds after being completely melted. In order to obtain alloy ingots with uniform components, all samples are repeatedly smelted for 5 times, and the samples are turned over after each smelting.
And 3, preparing the master alloy ingot into a strip with the width of 0.56mm and the thickness of 0.17 mu m in a vacuum strip-casting furnace.
And 4, cutting partial strips and performing cyclic treatment on the strips. The cycle parameters are set as: oil temperature 393K, cycle interval 1 minute, cycle number 15.
Comparative example 4
The chemical formula of the preparation is [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The iron-based amorphous alloy.
The preparation is as described in example 3, with the difference that no cooling-heating cycles are carried out.
The tensile properties at 693K were measured using a dynamic mechanical analyzer. FIG. 5 shows [ (Fe) prepared in comparative example 4 and example 4 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 Amorphous alloy tensile stress-strain curve. It can be seen that the tensile plasticity of the amorphous ribbon before cycling was 2.1% and that after cycling the tensile plasticity of the ribbon increased to 4%. Therefore, different cycle temperatures can improve the tensile plasticity of the iron-based amorphous alloy at different temperatures.
Example 5
And 2, distributing the weighed raw materials in a water-cooled copper mold crucible of the vacuum arc melting furnace in sequence according to the sequence of the melting points of the elements from low to high. Before smelting, the furnace chamber is vacuumized to 5 x 10 -3 Pa, and then filling argon to 0.7 atmosphere. During smelting, firstly smelting a titanium ingot in a furnace for 180 seconds to remove residual oxygen in a furnace cavity; when the target alloy is melted, the alloy is kept for 180 seconds after being completely melted. In order to obtain alloy ingots with uniform components, all samples are repeatedly smelted for 5 times, and the samples are turned over after each smelting.
And 3, preparing the master alloy ingot into a strip in a vacuum strip casting furnace.
And 4, respectively annealing the strips at 755K for 10/15/20 min, and then performing cold-hot circulation on the annealed samples, wherein the circulation temperature is 473K, the circulation interval time is 30 seconds, and the circulation times are 15 times.
Comparative example 5
The chemical formula of the preparation is [ (Fe) 0.5 Co 0.5 ) 0.75 B 0.2 Si 0.05 ] 96 Nb 4 The iron-based amorphous alloy.
The procedure is as in example 5, except that no cold-hot cycles are carried out after annealing.
The bending plasticity of comparative example 5 and example 5 is shown in fig. 6, the bending plasticity of the cycle samples after annealing is improved, and the improvement effect is more obvious when the annealing time is shorter. Coercivity as shown in fig. 7, the effect of cold-hot cycling on coercivity is almost negligible. When the annealing time is 15 minutes and the cold and hot cycles are carried out, the alloy coercive force is 3.8A/m and the bending plastic strain is 45 percent. Therefore, the iron-based amorphous soft magnetic alloy with excellent soft magnetic performance and bending plastic deformation capacity can be obtained by combining moderate annealing with a cold-hot cycle method.
Claims (10)
1. A method for improving the tensile plasticity of a toughened iron-based amorphous magnetically soft alloy strip is characterized in that the prepared iron-based amorphous magnetically soft alloy strip is subjected to cold-hot alternate circulation treatment; the temperature of the heat treatment is 0.4T g -0.6T g 。
2. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip according to claim 1, wherein the time of single cold treatment is 30s-3min.
3. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip according to claim 1, wherein in the step (2), the time of single heat treatment is 30s-3min.
4. The method for improving the tensile plasticity of the toughened iron-based amorphous soft magnetic alloy strip according to claim 1, wherein the number of the cold and hot alternating cycles is 10-30.
5. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip according to claim 1, wherein the interval time of the cold and hot alternating cycle is 30s-3min.
6. The method for improving the tensile plasticity of the toughened iron-based amorphous soft magnetic alloy strip according to claim 1, wherein the cold treatment process comprises the following steps: and (3) placing the iron-based amorphous magnetically soft alloy strip in liquid nitrogen.
7. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip according to claim 1, wherein the heat treatment process comprises the following steps: the iron-based amorphous soft magnetic alloy strip was placed in an oil bath.
8. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip according to claim 7, wherein the oil bath oil is polydimethylsiloxane.
9. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip as claimed in claim 1, wherein the iron-based amorphous magnetically soft alloy strip has a chemical formula of Fe in terms of atomic mol percent x Co y B 19.2 Si 4.8 Nb 4 Cu z Wherein x is more than or equal to 36 and less than or equal to 72, y is more than or equal to 0 and less than or equal to 36, z is more than or equal to 0 and less than or equal to 0.5, and x + y + z =72.
10. The method for improving the tensile plasticity of the toughened iron-based amorphous magnetically soft alloy strip according to claim 1, wherein the iron-based amorphous magnetically soft alloy strip is placed in a hollowed-out stainless steel ball, and then the hot and cold alternate cyclic treatment is performed.
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