EP4455355A1 - Amorphe/nanokristalline legierung auf eisenbasis und herstellungsverfahren dafür - Google Patents

Amorphe/nanokristalline legierung auf eisenbasis und herstellungsverfahren dafür Download PDF

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Publication number
EP4455355A1
EP4455355A1 EP22909121.0A EP22909121A EP4455355A1 EP 4455355 A1 EP4455355 A1 EP 4455355A1 EP 22909121 A EP22909121 A EP 22909121A EP 4455355 A1 EP4455355 A1 EP 4455355A1
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iron
amorphou
molten steel
nanocrystalline alloy
content
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French (fr)
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EP4455355A4 (de
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Jianwei BU
Jing PANG
Dong Yang
Fuqiang LIN
Wenkang YAO
Hongyu Liu
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Qingdao Yunlu Advanced Materials Technology Co Ltd
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Qingdao Yunlu Advanced Materials Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/003—Making ferrous alloys making amorphous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/02—Amorphous
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/04—Nanocrystalline

Definitions

  • the present invention relates to the technical field of magnetic materials, and specifically relates to an iron-based amorphou-nanocrystalline alloy and a preparation method thereof.
  • soft magnetic materials used as magnetic core, electric current transducer, magnetic sensor and pulse power magnetic component of transformer, motor or generator include silicon steel, ferrite, amorphous alloy and nanocrystalline alloy.
  • silicon steel is cheap, has high magnetic flux density and strong machinability, however, the loss becomes larger at a high frequency, so it is difficult to make the silicon steel sheet thinner in the thickness.
  • Ferrite has low saturation magnetic flux density, so the use of ferrite is limited under the condition of high power and high saturation magnetic induction.
  • Co-based amorphous alloy is not only expensive, but also has low saturation magnetic flux density, therefore, when used in a high-power device, the components will be enlarged, and its thermodynamics is unstable, and the loss increases during use.
  • Iron-based amorphous alloy has advantages both in saturation magnetic flux density and loss at high power, and it is the most ideal magnetic material, and thus the development of amorphous ferromagnetic alloys with high saturation magnetic induction intensity is urgent.
  • the main way to prepare this material is to increase the content of Fe in iron-based amorphous.
  • the thermal stability of the alloy decreases.
  • Sn, S, C, P and other elements are added.
  • the saturation magnetic induction intensity is increased by adding P to the amorphous Fe-Si-B-C-P system to increase the Fe content.
  • the patent also discloses that the long-term thermal stability is reduced due to the addition of P element, so the amorphous alloy in the above patent has not been manufactured by casting from their molten state.
  • An amorphous alloy strip with high saturation magnetic induction intensity is provided in Japanese patent disclosure No.2009052064 , which shows high thermal stability by adding Cr and Mn to control the height of the C deposition layer.
  • U.S. Patent No.7425239 mentions that Fe-Si-B-C is selected at a certain level of Si: C ratio, thus achieving magnetic properties in addition to high ductility.
  • the strip prepared by the above patents shows many defects on the surface, such as divisural line, slag line, scratch, inclusion and so on (as shown in Figures 1 and 2 ).
  • the technical problem solved by the present invention is to provide an iron-based amorphou-nanocrystalline alloy.
  • the iron-based amorphou-nanocrystalline alloy provided by the present application has high purity of molten steel, which can effectively improve the defects on the surface of the strip, effectively improve the lamination factor, and can obtain a product with excellent performance.
  • the atomic percent content of Fe ⁇ 83 Preferably, the atomic percent content of Fe ⁇ 83.
  • the impurity elements in the iron-based amorphou-nanocrystalline alloy are Al ⁇ 50ppm, Mn ⁇ 100ppm and Ti ⁇ 80ppm.
  • the iron-based amorphou-nanocrystalline alloy has a viscosity coefficient ⁇ of (3.0-8.0)* 10 -3 Pals.
  • d+ (b/c) 0.86-1.2
  • viscosity coefficient ⁇ is (4.1-6.9)* 10 -3 Pals.
  • the present application also provides a method of preparing the iron-based amorphou-nanocrystalline alloy, which comprises steps of: providing raw materials according to composition ratio, melting and calming each raw material, and then performing single-roller rapid quenching.
  • the calming is performed for a time of 30-50 min.
  • the present application ensures the control range of molten steel viscosity through the change of the content of the above alloying elements, so that the molten steel has a high purity, and thus ensures the continuity of the casting and the surface quality of strip.
  • the present invention mainly provides illustration on that molten steel containing P system is difficult to be manufactured by casting.
  • the reason why the iron-based amorphous alloy containing P is difficult to cast is the increase of P content.
  • the content of high melting point oxide element Si in molten steel decreases, so the content of low melting point oxide in molten steel increases, which is difficult to be separated from the molten steel, resulting in the oxide being discharged with molten steel in the form of slag during casting, so it is difficult to cast.
  • the present invention aims to improve the problem of strip surface defects caused by the poor thermal stability of the composition containing P, and the verified control means is to control the parameter ⁇ (i.e the dynamic viscosity of molten steel), so as to regulate the fluidity of molten steel, slag viscosity, etc., to obtain a liquid with very high purity of molten steel, thereby inhibiting the probability of strip surface defects from the source.
  • the parameter ⁇ i.e the dynamic viscosity of molten steel
  • the generation of the defect occurs at the beginning of the casting, and can continue with the extension of time, when the defect is sufficiently enlarged, cracks will be generated at the position of the defect, the process of crack initiation - growth - fracture leads to the stop of casting, which can also reduce the probability of the generation of defects in the first 30 minutes of casting by 70% and delay the time of defect generation to 1 h later, so as to effectively improve the pass rate of strip.
  • the strip with high saturation magnetic induction intensity can be obtained by casting, and the defects on the surface of the strip can be effectively improved to obtain excellent amorphous strip, thus effectively improve the lamination factor and obtain products with better performance in the manufacturing process of iron cores, transformers and other products in the application stage.
  • Fe is a ferromagnetic element, and in order to ensure the high saturation magnetic induction (BS, Bs ⁇ 1.75T in this application), the atomic percent of Fe should be greater than 83%, that is, (100-a-b-c-d-e) ⁇ 83.
  • Fe can improve the saturation magnetic induction intensity and reduce the material cost. If the Fe content is lower than 78at%, the expected saturation magnetic induction intensity cannot be achieved. If the Fe content is higher than 86 at%, it is difficult to form amorphous phase by quenching method, and coarse ⁇ -Fe crystal particle will be formed, and thus a uniform nanocrystalline structure cannot be obtained, resulting in a decline in soft magnetic properties.
  • Si can inhibit the precipitation of Fe and B compounds in the nanocrystalline structure after crystallization, thus stabilizing the nanocrystalline structure.
  • the content of Si is 0.2-6%.
  • the saturation magnetic induction intensity and amorphous forming ability will decrease, resulting in the deterioration of soft magnetic properties. It is especially pointed out that when the content of Si is above 0.8%, the amorphous forming ability will be improved and the thin strip can be produced stably and continuously.
  • Si is used as the forming element of high melting point oxides, which main functions are: forming slag with high melting point, which has good separability and can wrap low melting point oxides to float up and promote the purity of molten steel.
  • a layer of dense oxide film can be formed on the surface of molten steel to isolate the contact between molten steel and air, thus reducing the dynamic conditions for the formation of low melting point oxides.
  • the content of Si is 0.8-6%, and more preferably, the content of Si is 0.8-1.5%.
  • B as an essential element can improve the amorphous forming ability. If the content of B is less than 5%, it is difficult to form amorphous phase by quenching method. If the content of B is higher than 12%, it is not conducive to obtain uniform nanocrystalline structure, resulting in the decline of soft magnetic properties. In the present application, the content of B is 1%-12%. As a preferred embodiment, the content of B is 5-12%, and more preferably, the content of B is 8-12%.
  • P as an essential element can improve the amorphous forming ability. If the content of P is less than 1%, it is difficult to form amorphous phase by quenching method. If the content of P is higher than 8%, the saturation magnetic induction intensity decreases and the soft magnetic properties deteriorate. In the present application, the content of P is 2%-6%. When the content of P is 2-5%, the amorphous forming ability can be improved. More specifically, the content of P is 3-5%.
  • both elements B and P are the forming elements of low-melting-point oxides, and the separation effect of steel slag is bad.
  • Element C can increase the amorphous forming ability, and the addition of C can reduce the content of metalloid and reduce the material cost. If the content of C exceeds 5%, it will cause embrittlement and lead to decrease of soft magnetic properties. In particular, it is pointed out that when the content of C is less than 3%, the composition segregation caused by C volatilization can be suppressed. In this composition system, C can improve the activity of molten steel and promote the slagging reaction process.
  • Cu is beneficial to nanocrystallization, and when the content of Cu is lower than 0.6%, it is not conducive to nanocrystallization.
  • the content of Cu is 0.5-4%.
  • the content of Cu is 0.5-3%; more specifically, the content of Cu is 0.7-1.2%.
  • the content of Cu is higher than 1.4%, it will cause the nonuniformity of amorphous phase, which is not conducive to the formation of uniform nanocrystalline structure and leads to decrease of soft magnetic properties.
  • embrittlement of nanocrystalline alloys is considered, the Cu content should be controlled below 1.3%.
  • the content of Cu is conducive to the formation of a large number of fcc-Cu clusters and bcc-(Fe) crystal nucleus during quenching process, and at the same time promotes the precipitation of bcc-(Fe) crystal nucleus during heat treatment, thus improving the saturation magnetic induction intensity, and at the same time enabling the alloy to form a nanocrystalline structure with small crystal grain and uniform distribution in a wider temperature range of crystallization.
  • impurity elements Al, Mn and Ti heterogeneous nucleation will occur during the cooling process of molten steel, so the content of these elements is controlled by certain requirements: specifically, Al ⁇ 50ppm, Mn ⁇ 100ppm and Ti ⁇ 80ppm.
  • Ferromagnetic elements Co and Ni can replace part of Fe to maintain high Bs performance. Co can replace at most 15% of the atomic percent of Fe and Ni can replace at most 10% of the atomic percent of Fe.
  • the application regulates the element content through composition design, and further limits the viscosity coefficient according to the content of component, so as to control the composition of slag system, the proportion of component content in slag system, slag system state, slag tapping opportunity and slag weight through viscosity coefficient. Therefore, all oxides with low melting point that are difficult to slag in the molten steel can be precipitated, thereby improving the purity of molten steel and achieving the purpose of excellent casting characteristics of molten steel.
  • the surface defects of strip are caused by inclusions in molten steel, and the purity of molten steel is also controlled by this means.
  • the focuses herein is on how to establish the relationship between element content and dynamic viscosity ⁇ of molten steel through the element ratio, and how to regulate the dynamic viscosity coefficient ⁇ through the change of element content, so as to ensure the control range of viscosity of molten steel, and ensure the continuity of casting and the surface quality of the strip.
  • the viscosity, diffusion and conductivity rate of molten steel belong to the transmission properties of liquid, which are not only the basis for the study of the melt structure, but also the most important properties of smelting.
  • N, O and S can improve the viscosity of molten steel, and this effect often occurs at very low concentration of these elements.
  • the viscosity of molten steel is measured by damping vibration viscometer. In order to ensure the comparison of different components, the viscosity in the present application was measured at the same temperature of 1450 °C.
  • ⁇ the fluidity of molten steel is guaranteed within a certain range, thus the probability of surface defects of strip is suppressed from the source. Through this control, the casting time can be prolonged. The defect occurs at the initial stage of casting and will continue with the extension of time.
  • the probability of the generation of defects in the first 30 minutes of casting can be reduced by 70% and the time of defect generation can be delayed to 1 h later, so as to effectively improve the qualified rate of strip.
  • the defect of strip surface quality can be greatly improved, and the state of the surface slag line can be significantly improved, so that the frequency N of the slag line is reduced.
  • M the frequency of impurities within per unit area of 3mm*3mm
  • n the number of impurities * the height h (um) of impurities
  • the lamination factor of the strip can be greatly improved, from 84% to 89%.
  • the lamination factor has a great influence on the performance-loss of products.
  • the loss of strip products with high lamination factor can be reduced, and the loss of this component system can meet under the condition of 50 Hz and 1.5 T the Ps loss of iron core less than 0.35W/kg and the excitation Ss less than 0.4 ValKg.
  • the present application provides an iron-based amorphous alloy shown in the formula Fe (100-a-b-c-d-e) B a Si b P c C d Cu e , wherein, Fe, Si and B are beneficial to the formation of iron-based amorphous alloys with high saturation magnetic induction intensity.
  • the industrial raw materials required for the master alloy are pure Fe, pure Cu, elementary Si, pure C and Fe-B alloy and Fe-P alloy. The purity of raw materials is shown in Table 1. Table 1. Raw materials and their purity Raw materials Fe Cu Si C B-Fe (wt%-B) P-Fe (wt%-P) Purity % 99.95 99.99 99.6 99.95 17.94 24.32
  • the raw materials After weighing the raw materials according to the mass ratio, they are sequentially added into a medium frequency induction heating furnace for melting. Argon gas is introduced as a protective gas during the melting process, and after melting, the molten steel is calmed for 30 min to ensure that the composition of molten steel is uniform without segregation. After deoxidation, the viscosity of molten steel is measured using a damping vibration viscometer, with the measuring temperature set at 1450 °C. Then, the amorphous alloy ribbon is prepared by copper roller rapid quenching method: the molten steel is poured at 1400 °C-1500 °C, and the amorphous and nanocrystalline strip is obtained by copper roller rapid quenching method.
  • the length of time that defects begin to develop is recorded as a macro performance to measure the quality of molten steel.
  • the characteristics of slag line are analyzed by optical electron microscope, and the characteristics of impurity bulge are analyzed by a scanning electron microscope.
  • the performance of the strip is evaluated: the prepared amorphous and nanocrystalline strip is wound into a ring sample with the inner diameter of ⁇ 65 mm and the outer diameter of ⁇ 70 mm, and the performance of heat treatment is evaluated.
  • Performance evaluation and analysis are conducted after heat treatment.
  • the performance evaluation method is: 1) measurement of saturation magnetic induction intensity and coercivity: the saturation magnetization intensity Bs and coercivity of annealed alloy strip are measured by vibrating sample magnetometer (VSM) and soft magnetic DC tester. Based on the principle of electromagnetic induction, the equipment obtains the curve relationship between the sample magnetic moment and the external magnetic field, and the range of the test magnetic field is -10000 to 100000e. Before the test, the equipment is calibrated by using the prepared Ni reference material, and then the magnetic sample to be tested is crushed, weighed about 0.030 g, wrapped tightly with tinfoil, and placed in a copper mold for measurement.
  • VSM vibrating sample magnetometer
  • Each raw material was weighed according to the mass ratio, and then was sequentially added into a medium frequency induction heating furnace for melting.
  • Argon gas was introduced as a protective gas during the melting process, and after melting, the molten steel was calmed for 30 min to ensure that the composition of molten steel was uniform without segregation. After deoxidation, the viscosity of molten steel was measured by a damping vibration viscometer, and the measuring temperature is 1450 °C.
  • the elements that are strongly related to slag state were selected for analysis, that is, the main elements are four elements of Si, B, P and C.
  • the relationship between Si and ⁇ , and the relationship between Si and the related parameters of casting strip were mainly considered, so as to determine the element content and viscosity coefficient ⁇ under the performance advantage of strip.
  • Table 2 The specific implemented element ratio is shown in the following table 2: Table 2.
  • Si was used as the forming element of high melting point oxides, and it has the following functions: forming slag with high melting point, which has good separability and can wrap oxides with low melting point to float up and promote the purity of molten steel; in addition, forming a dense oxide film on the surface of molten steel to isolate the contact between molten steel and air, thus reducing the dynamic conditions for the formation of low melting point oxides.
  • the viscosity coefficient of molten steel increased obviously.
  • the content of Si is preferably in the range of 0.8-1.5%, the range of viscosity coefficient is 5.3-6.9 within this composition range , the time of casting defects is more than 50 min, the range of slag line is 80-120 and the range of M is 15-100. Because of the content of Si was low, the content of Fe in the comparative example s 1-3 was similar and high, and Bs had the advantage, but the slag state was more. When the content of Si was high, the slag state had advantage as a whole, but Bs was low due to the low content of Fe, and less than 1.75T could not meet the requirements.
  • Each raw material was weighed according to the mass ratio, and then was sequentially added into a medium frequency induction heating furnace for melting.
  • Argon gas was introduced as a protective gas during the melting process, and after melting, the molten steel was calmed for 30 min to ensure that the composition of molten steel was uniform without segregation. After deoxidation, the viscosity of molten steel was measured by a damping vibration viscometer, with the measuring temperature set at 1450 °C.
  • Example 3 the elements strongly related to slag state were selected for analysis, that is, the main elements are four elements of Si, B, P and C.
  • Example 2 the relationship between B and ⁇ , and the relationship between B and the related parameters of casting strip were mainly considered, so as to determine the element content and viscosity coefficient ⁇ under the performance advantage of strip.
  • Table 3 The specific implemented element ratio is shown in the following table 3: Table 3.
  • the slag of element B generated in the smelting process of molten steel was B 2 O 3 , which was an oxide with low melting point.
  • the content of element B had no great influence on the viscosity coefficient of molten steel, and the viscosity coefficient was relatively stable between 5%-7% when the atomic percent ratio of element B was 0%-15%.
  • the time of casting defects generation and performance indexes such as Bs
  • the content of B was lower than 8%
  • the amorphous forming ability of the system decreased
  • the amorphous degree of the strip decreased.
  • the Ps and Ss properties of the strip decreased under the same lamination factor.
  • the content of B was higher than 12%, the content of Fe decreased, and then Bs decreased to below 1.75T. Based on the above information, the content of B is finally limited to 8-12%.
  • Each raw material was weighed according to the mass ratio, and then was sequentially added into a medium frequency induction heating furnace for melting.
  • Argon gas was introduced as a protective gas during the melting process, and after melting, the molten steel was calmed for 30 min to ensure that the composition of molten steel was uniform without segregation. After deoxidation, the viscosity of molten steel was measured by a damping vibration viscometer, with the measuring temperature set at 1450 °C.
  • Example 3 the relationship between P and ⁇ , and the relationship between P and the related parameters of casting strip were mainly considered, so as to determine the element content and viscosity coefficient ⁇ under the performance advantage of strip.
  • Table 4 The specific implemented element ratio is shown in the following table 4: Table 4.
  • Each raw material was weighed according to the mass ratio, and then was sequentially added into a medium frequency induction heating furnace for melting.
  • Argon gas was introduced as a protective gas during the melting process, and after melting, the molten steel was calmed for 30 min to ensure that the composition of molten steel was uniform without segregation. After deoxidation, the viscosity of molten steel was measured by a damping vibration viscometer, with the measuring temperature set at 1450 °C.
  • Example 5 the elements strongly related to slag state were selected for analysis, that is, four main elements of Si, B, P and C.
  • Example 4 the relationship between C and ⁇ , and the relationship between C and the related parameters of casting strip were mainly considered, so as to determine the element content and viscosity coefficient ⁇ under the performance advantage of strip.
  • Table 5 The specific implemented element ratio is shown in the following table 5: Table 5.
  • element C did not participate in the reaction of slag formation in molten steel, and its main function was to improve the activity of element Si in molten steel, make the formation of oxides with high melting point was more thorough, improve the purity of molten steel and reduce the viscosity of molten steel, thus ensuring the fluidity of molten steel.
  • the viscosity coefficient of molten steel was 10.2
  • the fluidity of molten steel was poor, the defects occured earlier in the casting process, and there were many slag lines and impurity defects in the strip, and the corresponding lamination factor was low, which led to the final performance deteriorated.
  • the quality of molten steel was obviously improved, the viscosity was reduced, the fluidity was increased, and there were fewer oxides such as slag in molten steel. Therefore, the quality of the strip was improved and the performance was improved correspondingly.
  • the content of C was finally selected at 0.7-0.9%.
  • Example 5 the relationship between mutual coupling of main elements and ⁇ , and the relationship between mutual coupling of main elements and the related parameters of casting strip were mainly considered, so as to determine the element content and viscosity coefficient ⁇ under the performance advantage of strip.
  • Table 6 The specific implemented element ratio is shown in the following table 6: Table 6.

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EP22909121.0A 2021-12-22 2022-05-10 Amorphe/nanokristalline legierung auf eisenbasis und herstellungsverfahren dafür Pending EP4455355A4 (de)

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CN202111583663.7A CN114250426B (zh) 2021-12-22 2021-12-22 一种铁基非晶纳米晶合金及其制备方法
PCT/CN2022/091867 WO2023115785A1 (zh) 2021-12-22 2022-05-10 一种铁基非晶纳米晶合金及其制备方法

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CN115386811B (zh) * 2022-09-26 2023-11-17 安徽工业大学芜湖技术创新研究院 一种高饱和磁感应强度韧性铁基非晶纳米晶带材

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CN114250426B (zh) * 2021-12-22 2022-10-11 青岛云路先进材料技术股份有限公司 一种铁基非晶纳米晶合金及其制备方法

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