CN115927978A - Low-loss high-magnetic-flux-density iron-based amorphous soft magnetic alloy and preparation method thereof - Google Patents
Low-loss high-magnetic-flux-density iron-based amorphous soft magnetic alloy and preparation method thereof Download PDFInfo
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- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 65
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- 229910045601 alloy Inorganic materials 0.000 claims abstract description 158
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Abstract
The invention discloses a low-loss high-magnetic-flux-density iron-based amorphous soft magnetic alloy and a preparation method thereof, wherein the formula of the soft magnetic alloy is as follows: fe a Co b B c Si d C e P f Cu g A, b, c, d, e, f and g respectively represent atomic percentages of corresponding alloy elements and satisfy the following conditions: 67 is less than or equal to a<83，0<b≤16，9≤c≤10，2≤d≤5，0≤e≤3，0<f≤4，0≤g≤1，a:b≥4，81<a+b<84, a, b, c, d, e, f, g, and 100. The preparation method comprises the following steps: the method comprises the steps of carrying out induction melting on raw materials under a protective atmosphere to obtain a master alloy ingot, preparing an amorphous alloy strip by adopting a single-roll quenching method, and carrying out tensile stress heat treatment under a vacuum condition or in an inert atmosphere to obtain the amorphous alloy strip. After the alloy is subjected to tensile stress heat treatment, the soft magnetic performance of the alloy is greatly improved, the saturation magnetic flux density reaches 1.8T, and the coercive force is 1.8-2.5A/m.
Description
Technical Field
The invention relates to an amorphous soft magnetic alloy and a preparation method thereof, in particular to a low-loss high-magnetic-flux-density iron-based amorphous soft magnetic alloy and a preparation method thereof.
Background
At present, the saturation magnetic flux density of the iron-based amorphous soft magnetic alloy is still obviously lower than that of silicon steel, and the development of the amorphous soft magnetic alloy with high saturation magnetic flux density and low iron loss has important significance for realizing miniaturization, energy conservation and high efficiency of electronic components. Researchers have developed a plurality of studies around component design and process optimization to develop high saturation magnetic flux density and low loss iron-based amorphous soft magnetic alloy.
Patent CN101552071B discloses an iron-based amorphous soft magnetic alloy and a preparation method thereof, wherein the amorphous alloy comprises the following chemical components: fe a P b B c C d Si e The saturation magnetic induction intensity is 1.45-1.70T, the coercive force is 3-5A/m, and the Curie temperature is 568-593K, the iron-based amorphous soft magnetic alloy disclosed by the patent is in a bar form, and the preparation method does not comprise a heat treatment process. Patent CN109778083B discloses a high saturation induction density Fe-based amorphous alloy and a preparation method thereof, the chemical expression of the alloy is Fe (a-x) -Co (x) -B (B) -C (C) -Si (d) -P (e) -M (f), the saturation induction density is 1.58-1.83T, and the coercive force is 1-8.7A/M. The heat treatment methods disclosed in this patent are ordinary heat treatment and magnetic field heat treatment.
The cobalt doping is one of means for improving the saturation magnetic flux density of the alloy, has the advantages of high efficiency and easy implementation, and does not deteriorate the amorphous forming capability and the processing performance of the alloy. However, for a FeCo-based amorphous alloy with a high curie temperature, soft magnetic performance is deteriorated due to stress relief heat treatment in a ferromagnetic state, and a magnetic domain structure is usually regulated and controlled by using uniaxial magnetic anisotropy induced by an external magnetic field along an external magnetic field direction to optimize the soft magnetic performance. And when the magnetic field heat treatment is carried out above or near the curie temperature, the improvement of the soft magnetic property is small compared with the common heat treatment.
Patent CN105648158B discloses a device and method for improving the magnetic performance of amorphous alloy soft magnetic material, the method adopts low temperature stress annealing technology, that is, annealing technology combining the action of axial tensile stress below the crystallization temperature, to obviously improve the maximum giant magneto-impedance ratio of the amorphous alloy thin bands of FeCuNbSiB, feconnbsib, fesiccu. The patent is limited to the optimization of magnetic properties, which is the giant magneto-impedance effect.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a low-loss high-flux density iron-based amorphous soft magnetic alloy with excellent and controllable comprehensive soft magnetic performance;
the second purpose of the invention is to provide a preparation method of the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density.
The technical scheme is as follows: the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density has the molecular formula as follows: fe a Co b B c Si d C e P f Cu g Wherein a, b, c, d, e, f and g respectively represent atomic percentages of corresponding alloy elements and satisfy the following conditions: 67 is more than or equal to a<83，0<b≤16，9≤c≤10，2≤d≤5，0≤e≤3，0<f≤4，0≤g≤1，a:b≥4，81<a+b<84，a+b+c+d+e+f+g＝100。
Wherein the Curie temperature range of the iron-based amorphous soft magnetic alloy is 606-750K.
The iron-based amorphous alloy has a saturation magnetic flux density of 1.67-1.80T, a coercive force of less than 2.5A/m, loss of less than 0.11W/kg under the conditions of 50Hz and 1.0T, loss of no more than 0.17W/kg under the conditions of 50Hz and 1.5T, and effective magnetic permeability of 27000-33000 under the conditions of 1kHz and 5A/m.
The preparation method of the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density comprises the following steps:
(1) Weighing the raw materials according to the atomic percentage;
(2) Carrying out induction melting on the prepared raw materials under a protective atmosphere, and cooling to obtain a master alloy ingot with uniform components;
(3) Preparing the master alloy ingot into an amorphous alloy strip by adopting a single-roll quenching method;
(4) And carrying out tensile stress heat treatment on the amorphous alloy strip under a vacuum condition or in an inert atmosphere to obtain the iron-based amorphous soft magnetic alloy with optimized performance.
In the step (4), the method for applying tensile stress by the tensile stress heat treatment comprises the following steps: cutting the amorphous alloy strip by 4-18cm, fixing two ends of the amorphous alloy strip, and applying axial stress to the strip by 50-250MPa. In order to meet the requirement of magnetic conductivity test on the size of a sample and ensure the uniform stress of the strip, the length of the strip is preferably 4-18cm, and in order to obtain excellent soft magnetic performance and avoid the strip from breaking, the applied stress is preferably 50-250MPa.
In the step (4), the temperature raising and reducing method of the tensile stress heat treatment comprises the following steps: and sliding the furnace body heated to the preset temperature of 573-713K to the position of the sample, preserving the temperature for 10-20min, and then cooling. In order to sufficiently eliminate residual internal stress and avoid crystallization from high-temperature long-time heat treatment to deteriorate soft magnetic properties, the heat treatment temperature and time are preferably 573-713K and 10-20min.
Wherein, in the step (4), the tensile stress heat treatment is carried out at a temperature lower than the crystallization temperature; the tensile stress is optimally matched with the heat treatment temperature and the heat treatment time, so that the soft magnetic performance of the amorphous alloy is obviously improved.
In the step (4), the tensile stress heat treatment method promotes the iron-based amorphous alloy to form a regular magnetic domain and regulates and controls the magnetic domain to be arranged along the tensile stress direction, and the width of the magnetic domain is 150-200 μm; the domain wall is flat and smooth, and the magnetization mechanism is mainly transformed from non-uniform domain rotation to uniform domain wall displacement.
In the step (4), in order to ensure that the belt-making process realizes deep undercooling and quenching and simultaneously improves the surface quality of the belt material, the single-roller quenching method comprises the following process parameters: the spraying pressure is 0.01-0.03MPa, and the surface linear velocity of the copper roller is 30-50m/s.
The invention principle is as follows: the invention is based on the use of amorphous soft magnetic materialsAccording to scientific research experience in the field of materials, a large number of experiments show that the addition of Co element is beneficial to improving the saturation magnetic flux density and Curie temperature of the iron-based amorphous alloy and improving the temperature stability of the amorphous soft magnetic alloy, but the excessive Co addition can reduce the saturation magnetic flux density and increase the raw material cost. The invention selects Fe-based amorphous alloy component Fe with large amorphous forming capability and high thermal stability 83 B 10 Si 3 C 3 P 1 On the basis, the content of Co element is optimized. The tensile stress heat treatment in the invention promotes the formation of regular magnetic domains and regulates the orientation of the magnetic domains, the magnetic domains are arranged along the tensile stress direction, and the width is 150-200 μm. The application of tensile stress during the heat treatment causes the magnetization mechanism to switch from being dominated by non-uniform domain rotation to being dominated by uniform domain wall displacement. The tensile stress heat treatment of the invention has certain universality for obviously improving the soft magnetic performance of the amorphous alloy and is not restricted by the Curie temperature of the amorphous alloy.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: (1) The iron-based amorphous alloy provided by the invention has excellent and controllable comprehensive soft magnetic performance, the saturation magnetic flux density is 1.67-1.80T, the coercive force is 1.86-2.49A/m, the effective magnetic conductivity is 27000-33000 under the conditions of 1kHz and 5A/m, the loss is 0.10-0.11W/kg under the conditions of 50Hz and 1.0T, the loss is not more than 0.17W/kg under the conditions of 50Hz and 1.5T, the power frequency loss is equivalent to that of a commercial METGLAS2605S2 amorphous soft magnetic alloy, wherein the saturation magnetic flux density of the commercial METGLAS2605S2 is 1.54T. (2) The iron-based amorphous soft magnetic alloy provided by the invention has a wide Curie temperature range of 606K to 707K, the distance between the first crystallization peak and the second crystallization peak is 120-135K, and the iron-based nanocrystalline soft magnetic alloy can be prepared by a nano crystallization heat treatment process by utilizing the characteristic of wide distance between the first crystallization peak and the second crystallization peak. (3) On the basis of the alloy components, the iron-based amorphous soft magnetic alloy is prepared by combining a tensile stress heat treatment method, the process is simple, the curie temperature of the alloy is not restricted, the applicability is wide, the heat treatment temperature is low, the method has the advantages of reducing the production energy consumption and cost and improving the production efficiency, and the application prospect is wide.
Drawings
FIG. 1 is an X-ray diffraction pattern of quenched alloy ribbons prepared in examples 1-4;
FIG. 2 is a DSC curve of a ribbon of quenched alloy prepared in examples 1-4;
FIG. 3 is a graph showing the change in permeability and coercivity of example 2 and comparative example 2 after 20 minutes of incubation at 573-673K;
FIG. 4 is a graph showing the change in loss after holding the optimal heat treatment temperature for 20 minutes for examples 1 to 4 and comparative examples 1 to 4;
FIG. 5 is an X-ray diffraction pattern of example 2 and comparative example 2 after 20 minutes of incubation at the optimum heat treatment temperature;
FIG. 6 is a magnetic domain structure image of example 2 after 20 minutes of incubation at the optimum heat treatment temperature;
fig. 7 is a magnetic domain structure image of comparative example 2 after 20 minutes of incubation at the optimum heat treatment temperature.
Detailed Description
The present invention is described in further detail below.
Example 1
Molecular formula of Fe 79 Co 4 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atom percentage to obtain 15g of a mixture, wherein the mass percentage of carbon in the iron-carbon intermediate alloy is 5%, and the mass percentage of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then turning off a heating power supply, cooling an alloy melt to 1350K, and carrying out melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear velocity of a copper roller of 30m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; wherein the injection pressure is 0.01MPa;
(4) Cutting 4cm of the prepared amorphous alloy strip, fixing the amorphous alloy strip in a self-made clamp, applying axial stress of 50MPa to the strip by a special rectangular weight, putting the amorphous alloy strip into a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 multiplied by 10 -3 Pa; and when the temperature of the heat treatment furnace reaches a preset value 653K, sliding the furnace body to the position of the sample, preserving the heat for 10 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Example 2
Molecular formula of Fe 75 Co 8 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atom percentage to obtain 15g of a mixture, wherein the mass percentage of carbon in the iron-carbon intermediate alloy is 5%, and the mass percentage of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a master alloy ingot, then loading the crushed master alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1350K, and spinning the alloy melt by adopting a single-roller quenching spinning technology at the surface linear velocity of a copper roller of 40m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; wherein the injection pressure is 0.03MPa;
(4) Cutting 6cm from the prepared amorphous alloy strip, fixing in a self-made fixture, applying axial stress 150MPa to the strip by a special rectangular weight, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Example 3
Molecular formula of Fe 71 Co 12 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atom percentage to obtain 15g of a mixture, wherein the mass percentage of carbon in the iron-carbon intermediate alloy is 5%, and the mass percentage of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1400K, and spinning at the surface linear velocity of a copper roller of 50m/s by adopting a single-roller quenching and spinning technology to prepare an amorphous alloy strip with the width of 1mm and the thickness of 20 mu m; the injection pressure is 0.03MPa;
(4) Cutting 18cm from the prepared amorphous alloy strip, fixing in a self-made fixture, applying axial stress of 250MPa to the strip by a special rectangular weight, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches a preset value 573K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away from the furnace body, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Example 4
Molecular formula of Fe 67 Co 16 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atom percentage to obtain 15g of a mixture, wherein the mass percentage of carbon in the iron-carbon intermediate alloy is 5%, and the mass percentage of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling the alloy melt to 1400K, and spinning the alloy melt by adopting a single-roller quenching spinning technology at the surface linear speed of a copper roller of 40m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 22 mu m; wherein the injection pressure is 0.03MPa;
(4) Cutting 10cm of the prepared amorphous alloy strip, fixing the amorphous alloy strip in a self-made clamp, applying axial stress of 50MPa to the strip by a special rectangular weight, putting the amorphous alloy strip into a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 multiplied by 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
The quenched alloy strips obtained in step (3) of examples 1 to 4 were tested for structure by an X-ray diffractometer, and as a result, as shown in FIG. 1, all the quenched alloy samples were obtained with only one dispersion diffraction peak, indicating that they were amorphous structures.
The thermal property parameters of the quenched alloy strip obtained in the step (3) of examples 1 to 4 were measured by a differential scanning calorimeter, and the initial crystallization temperature T was measured at a temperature rise rate of 40K/min x1 The second crystallization temperature T x2 And Curie temperature T C As shown in fig. 2. T of alloy strip x1 Is 703-711K, T x2 831 to 838K, T C The temperature range of the heat treatment is determined to be 662K to 707K, and the temperature range of the heat treatment is determined to be 573-653K.
Example 5
Molecular formula of Fe 77.2 Co 4 Si 4.5 B 9.5 P 4 Cu 0.8 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Proportioning raw materials of iron, cobalt, boron, silicon, copper and iron-phosphorus master alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of phosphorus in the iron-phosphorus master alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a master alloy ingot, then loading the crushed master alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1350K, and spinning at the surface linear velocity of a copper roller of 40m/s by adopting a single-roller quenching spinning technology to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; the injection pressure is 0.03MPa;
(4) Cutting 6cm from the prepared amorphous alloy strip, fixing in a self-made fixture, applying axial stress of 50MPa to the strip by a special rectangular weight, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches a preset value of 713K, sliding the furnace body to the position of the sample, preserving the heat for 10 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Example 6
Molecular formula of Fe 79.2 Co 4 Si 2.5 B 9.5 P 4 Cu 0.8 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Proportioning raw materials of iron, cobalt, boron, silicon, copper and iron-phosphorus master alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of phosphorus in the iron-phosphorus master alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then turning off a heating power supply, cooling an alloy melt to 1350K, and spinning at the surface linear speed of a copper roller of 40m/s by adopting a single-roller quenching and spinning technology to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; the injection pressure is 0.03MPa;
(4) Cutting 8cm of the prepared amorphous alloy strip, fixing the amorphous alloy strip in a self-made clamp, applying axial stress of 50MPa to the strip by a special rectangular weight, putting the amorphous alloy strip into a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 multiplied by 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Example 7
Molecular formula of Fe 67.2 Co 16 Si 2.5 B 9.5 P 4 Cu 0.8 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, copper and iron-phosphorus master alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of phosphorus in the iron-phosphorus master alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1400K, and spinning at the surface linear velocity of a copper roller of 50m/s by adopting a single-roller quenching and spinning technology to prepare an amorphous alloy strip with the width of 1mm and the thickness of 20 mu m; wherein the injection pressure is 0.02MPa;
(4) Cutting 10cm of the prepared amorphous alloy strip, fixing the amorphous alloy strip in a self-made clamp, applying axial stress of 50MPa to the strip by a special rectangular weight, putting the amorphous alloy strip into a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 multiplied by 10 -3 Pa; when the temperature of the heat treatment furnace reaches 633K, the furnace body is slid to the position of the sample, the temperature is preserved for 20 minutes, and then the furnace body is slid away from the furnace body and the sample is cooled by an electric fan to obtain the productTo iron-based amorphous soft magnetic alloys.
Comparative examples 1 to 7 were set as follows, and are different from examples 1 to 7 in that only the ordinary heat treatment was performed in step (4), and the effects of the tensile stress heat treatment method and the ordinary heat treatment method on the soft magnetic properties of the amorphous alloy were analyzed and compared.
Comparative example 1
Molecular formula of Fe 79 Co 4 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atom percentage to obtain 15g of a mixture, wherein the mass percentage of carbon in the iron-carbon intermediate alloy is 5%, and the mass percentage of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a master alloy ingot, then loading the crushed master alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1350K, and performing melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear velocity of a copper roller of 30m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; wherein the injection pressure is 0.01MPa.
(4) Cutting 4cm from the prepared amorphous alloy strip, fixing in a self-made clamp without applying axial stress, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches a preset value 653K, sliding the furnace body to the position of the sample, preserving the heat for 10 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Comparative example 2
Molecular formula of Fe 75 Co 8 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atom percentage to obtain 15g of a mixture, wherein the mass percentage of carbon in the iron-carbon intermediate alloy is 5%, and the mass percentage of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a master alloy ingot, then loading the crushed master alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1350K, and carrying out melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear velocity of a copper roller of 40m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; wherein the injection pressure is 0.03MPa;
(4) Cutting 6cm from the prepared amorphous alloy strip, fixing in a self-made clamp without applying axial stress, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Comparative example 3
Molecular formula of Fe 71 Co 12 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Proportioning raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of carbon in the iron-carbon intermediate alloy is 5%, and the mass percent of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1400K, and performing melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear velocity of a copper roller of 50m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 20 mu m; wherein the injection pressure is 0.03MPa;
(4) Cutting 18cm from the prepared amorphous alloy strip, fixing in a self-made clamp without applying axial stress, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches a preset value 573K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away from the furnace body, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Comparative example 4
Molecular formula of Fe 67 Co 16 B 10 Si 3 C 3 P 1 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Proportioning raw materials of iron, cobalt, boron, silicon, an iron-carbon intermediate alloy and an iron-phosphorus intermediate alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of carbon in the iron-carbon intermediate alloy is 5%, and the mass percent of phosphorus in the iron-phosphorus intermediate alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then turning off a heating power supply, cooling the alloy melt to 1400K, and performing melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear speed of a copper roller of 40m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 22 mu m; wherein the injection pressure is 0.03MPa;
(4) Cutting 10cm from the prepared amorphous alloy strip, fixing the amorphous alloy strip on a self-made clamp, applying no axial stress, placing the amorphous alloy strip into a quartz tube matched with a heat treatment furnace, and pumpingVacuum to 5X 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Comparative example 5
Molecular formula of Fe 77.2 Co 4 Si 4.5 B 9.5 P 4 Cu 0.8 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Proportioning raw materials of iron, cobalt, boron, silicon, copper and iron-phosphorus master alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of phosphorus in the iron-phosphorus master alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then turning off a heating power supply, cooling an alloy melt to 1350K, and carrying out melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear speed of a copper roller of 40m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; the injection pressure is 0.03MPa;
(4) Cutting 6cm from the prepared amorphous alloy strip, fixing in a self-made clamp without applying axial stress, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches a preset value of 713K, sliding the furnace body to the position of the sample, preserving the heat for 10 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Comparative example 6
Molecular formula of Fe 79.2 Co 4 Si 2.5 B 9.5 P 4 Cu 0.8 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, copper and iron-phosphorus master alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of phosphorus in the iron-phosphorus master alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a master alloy ingot, then loading the crushed master alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then closing a heating power supply, cooling an alloy melt to 1350K, and carrying out melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear velocity of a copper roller of 40m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 23 mu m; wherein the injection pressure is 0.03MPa;
(4) Cutting 8cm from the prepared amorphous alloy strip, fixing in a self-made clamp without applying axial stress, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
Comparative example 7
Molecular formula of Fe 67.2 Co 16 Si 2.5 B 9.5 P 4 Cu 0.8 The preparation method of the iron-based amorphous soft magnetic alloy comprises the following steps:
(1) Mixing raw materials of iron, cobalt, boron, silicon, copper and iron-phosphorus master alloy according to atomic percent to obtain 15g of a mixture, wherein the mass percent of phosphorus in the iron-phosphorus master alloy is 26.4%;
(2) Smelting the prepared mixture by using an induction smelting furnace under the protection of argon to obtain a master alloy ingot with uniform components;
(3) Crushing a mother alloy ingot, then loading the crushed mother alloy ingot into a quartz tube with a nozzle at the bottom, fixing the quartz tube in an induction coil, under the protection of high-purity argon, rapidly melting the small alloy ingot by induction heating, then turning off a heating power supply, cooling the alloy melt to 1400K, and performing melt spinning by adopting a single-roller quenching melt spinning technology at the surface linear velocity of a copper roller of 50m/s to prepare an amorphous alloy strip with the width of 1mm and the thickness of 20 mu m; the injection pressure is 0.02MPa;
(4) Cutting 10cm from the prepared amorphous alloy strip, fixing in a self-made clamp without applying axial stress, placing in a quartz tube matched with a heat treatment furnace, and vacuumizing to 5 × 10 -3 Pa; and when the temperature of the heat treatment furnace reaches 633K, sliding the furnace body to the position of the sample, preserving the heat for 20 minutes, then sliding the furnace body away, and cooling the sample by using an electric fan to obtain the iron-based amorphous soft magnetic alloy.
And measuring the magnetic permeability of the alloy sample by adopting an impedance analyzer under the conditions of 1kHz and 5A/m, and measuring the coercive force of the alloy sample by adopting a direct-current hysteresis loop measuring instrument under a 1kA/m magnetic field. The measurement results of the quenched alloy sample in example 2, the alloy sample after the tensile stress heat treatment and the comparative example 2 are shown in fig. 3, and it can be seen that the example 2 after the tensile stress heat treatment has good soft magnetic performance in the temperature range of 573-653K, the magnetic permeability is greatly improved, the coercive force is less than 5A/m, and the magnetic permeability of the quenched alloy sample is reduced and the coercive force is obviously increased compared with the quenched alloy sample in the comparative example 2. The example 2 obtained the optimum soft magnetic properties when the heat treatment temperature was 633K, and the soft magnetic properties of both the example 2 and the comparative example 2 were significantly deteriorated when the heat treatment temperature was increased to 673K.
The loss of the alloy sample was measured under the conditions of 1.0T and 50Hz by using an AC hysteresis loop measuring apparatus, and the measurement results of the quenched alloy samples of examples 1 to 4, the alloy samples after the tensile stress heat treatment and comparative examples 1 to 4 are shown in FIG. 4. It is understood that the power frequency loss after the tensile stress heat treatment at the optimum heat treatment temperature is reduced to 0.11W/kg or less in examples 1 to 4, while the power frequency loss is only slightly reduced in comparative example 1 as compared with the quenched sample, and the power frequency loss is even further increased in comparative examples 3 and 4 as compared with the quenched sample.
Description accompanying Table 1 details the permeability, coercive force, loss and saturation magnetic flux density of the alloy samples subjected to the tensile stress heat treatment at the optimum heat treatment temperature in examples 1 to 7 and the alloy samples subjected to the ordinary heat treatment at the optimum heat treatment temperature in comparative examples 1 to 7, the saturation magnetic flux density being measured at a magnetic field of 800kA/m using a vibrating sample magnetometer. The series of Fe-based amorphous alloysAfter being optimized by tensile stress heat treatment, the gold has excellent comprehensive soft magnetic performance, the saturation magnetic flux density is 1.67-1.80T, the coercive force is 1.86-2.49A/m, the effective magnetic conductivity is 27000-33000 under the conditions of 1kHz and 5A/m, and the loss is 0.10-0.11W/kg under the conditions of 50Hz and 1.0T. The symbols in table 1 have the following meanings: mu.s e For effective permeability, H c Is coercive force, P 10/50 Is a loss under the conditions of 1.0T and 50Hz, B s Is the saturation magnetic flux density.
TABLE 1
The phase structure of the alloy strip after the tensile stress heat treatment and the ordinary heat treatment is also tested by an X-ray diffractometer. The X-ray diffraction patterns of the alloy strip after the tensile stress heat treatment at the optimum heat treatment temperature in example 2 and the alloy strip after the ordinary heat treatment at the optimum heat treatment temperature in comparative example 2 are shown in fig. 5, and the alloy strip samples prepared by different heat treatment methods have only one dispersion diffraction peak, which indicates that the amorphous structure is still maintained.
The magnetization process of the alloy sample was observed by using a magneto-optical kerr microscope, and the dynamic magnetic domain evolution of the alloy sample after the tensile stress heat treatment at the optimum heat treatment temperature in example 2 is shown in fig. 6. The alloy after the tensile stress heat treatment has regular magnetic domain arrangement, basically consistent orientation and tensile stress direction, width over 150 microns, flat and smooth domain wall, no obvious pinning point and magnetizing mechanism dominated by uniform domain wall displacement. The dynamic magnetic domain evolution of the alloy sample subjected to the ordinary heat treatment at the optimum heat treatment temperature in the comparative example 2 is shown in fig. 7, and it can be seen that the magnetic domain of the alloy subjected to the ordinary heat treatment is narrow and irregular, and is branched, the magnetization process is dominated by the rotation of the non-uniform magnetic domain, and the domain wall pinning effect is strong along with a small amount of domain wall displacement.
In summary, the present invention provides a low-loss high-flux-density fe-based amorphous soft magnetic alloy, which has a wide curie temperature range of 606K to 707K or higher; the invention also provides a preparation method of the amorphous soft magnetic alloy, namely tensile stress heat treatment is carried out on the amorphous alloy strip, so that the effective regulation and control of soft magnetic performance are realized, and the optimal matching of heat treatment temperature and time and tensile stress is determined through a large number of experiments, so that the alloy has excellent comprehensive soft magnetic performance. The embodiment shows that the saturation magnetic flux density of the iron-based amorphous soft magnetic alloy is 1.67-1.80T, the coercive force is 1.86-2.49A/m, the effective magnetic conductivity under the conditions of 1kHz and 5A/m is 27000-33000, and the loss under the conditions of 50Hz and 1.0T is 0.10-0.11W/kg; the tensile stress heat treatment method has the advantages of simple process, no restriction of Curie temperature, wide applicability, lower heat treatment temperature, reduction of production energy consumption and cost, improvement of production efficiency and wide application prospect.
Claims (9)
1. The iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density is characterized in that the molecular formula of the iron-based amorphous soft magnetic alloy is as follows: fe a Co b B c Si d C e P f Cu g Wherein a, b, c, d, e, f and g respectively represent the atomic percent of the corresponding alloy elements and satisfy the following conditions: 67 is less than or equal to a<83，0<b≤16，9≤c≤10，2≤d≤5，0≤e≤3，0<f≤4，0≤g≤1，a:b≥4，81<a+b<84，a+b+c+d+e+f+g＝100。
2. The low-loss high-flux-density fe-based amorphous soft magnetic alloy according to claim 1, wherein the fe-based amorphous soft magnetic alloy has a curie temperature in the range of 606K-750K.
3. The low loss high flux density fe-based amorphous soft magnetic alloy according to claim 1, wherein the fe-based amorphous alloy has a saturation flux density of 1.67-1.80T, a coercivity below 2.5A/m, a loss of less than 0.11W/kg at 50Hz and 1.0T, a loss of no more than 0.17W/kg at 50Hz and 1.5T, and an effective permeability of 27000-33000 at 1kHz and 5A/m.
4. The method for preparing the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density according to claim 1, which comprises the following steps:
(1) Weighing the raw materials according to the atomic percentage;
(2) Carrying out induction melting on the prepared raw materials under a protective atmosphere, and cooling to obtain a master alloy ingot with uniform components;
(3) Preparing the master alloy ingot into an amorphous alloy strip by adopting a single-roll quenching method;
(4) And carrying out tensile stress heat treatment on the amorphous alloy strip under a vacuum condition or in an inert atmosphere to obtain the iron-based amorphous soft magnetic alloy.
5. The method for preparing the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density according to claim 4, wherein in the step (4), the tensile stress is applied by the following method: cutting the amorphous alloy strip by 4-18cm, fixing two ends of the amorphous alloy strip, and applying axial stress to the strip by 50-250MPa.
6. The method for preparing the low-loss high-flux-density iron-based amorphous soft magnetic alloy according to claim 4, wherein in the step (4), the temperature rising and reducing method of the tensile stress heat treatment comprises the following steps: and sliding the furnace body heated to the preset temperature of 573-713K to the position of the sample, preserving the temperature for 10-20min, and then cooling.
7. The method for preparing low-loss high-flux density Fe-based amorphous soft magnetic alloy according to claim 4, wherein in the step (4), the tensile stress heat treatment is performed at a temperature lower than the crystallization temperature.
8. The method for preparing the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density according to claim 4, wherein in the step (4), the tensile stress heat treatment method promotes the iron-based amorphous alloy to form regular magnetic domains and regulates the arrangement of the magnetic domains along the tensile stress direction, and the magnetic domain width is 150-200 μm.
9. The method for preparing the iron-based amorphous soft magnetic alloy with low loss and high magnetic flux density according to claim 4, wherein in the step (4), the process parameters of the single-roll quenching method are as follows: the spraying pressure is 0.01-0.03MPa, and the surface linear velocity of the copper roller is 30-50m/s.
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| CN104073749A (en) * | 2014-06-18 | 2014-10-01 | 安泰科技股份有限公司 | Iron-based amorphous magnetically soft alloy with uniform element distribution and preparation method thereof |
| JP2015157999A (en) * | 2014-02-25 | 2015-09-03 | 国立大学法人東北大学 | ALLOY COMPOSITION, Fe-BASED NANO-CRYSTAL ALLOY RIBBON, Fe-BASED NANO-CRYSTAL ALLOY POWDER AND MAGNETIC PART |
| CN105648158A (en) * | 2016-01-14 | 2016-06-08 | 浙江师范大学 | Device and method for improving magnetic performance of amorphous alloy soft magnetic material |
| CN110993239A (en) * | 2019-04-19 | 2020-04-10 | 东南大学 | Iron-cobalt-based amorphous soft magnetic alloy and preparation method thereof |
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| JP2015157999A (en) * | 2014-02-25 | 2015-09-03 | 国立大学法人東北大学 | ALLOY COMPOSITION, Fe-BASED NANO-CRYSTAL ALLOY RIBBON, Fe-BASED NANO-CRYSTAL ALLOY POWDER AND MAGNETIC PART |
| CN104073749A (en) * | 2014-06-18 | 2014-10-01 | 安泰科技股份有限公司 | Iron-based amorphous magnetically soft alloy with uniform element distribution and preparation method thereof |
| CN105648158A (en) * | 2016-01-14 | 2016-06-08 | 浙江师范大学 | Device and method for improving magnetic performance of amorphous alloy soft magnetic material |
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