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US20210198761A1 - Iron-based amorphous alloy and method for preparing the same - Google Patents

Iron-based amorphous alloy and method for preparing the same Download PDF

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Publication number
US20210198761A1
US20210198761A1 US16/065,670 US201716065670A US2021198761A1 US 20210198761 A1 US20210198761 A1 US 20210198761A1 US 201716065670 A US201716065670 A US 201716065670A US 2021198761 A1 US2021198761 A1 US 2021198761A1
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Prior art keywords
iron
based amorphous
amorphous alloy
strip
present disclosure
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Inventor
Xiaoyu Li
Jing Pang
Qinghua Li
Dong Yang
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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Assigned to QINGDAO YUNLU ADVANCED MATERIALS TECHNOLOGY CO., LTD. reassignment QINGDAO YUNLU ADVANCED MATERIALS TECHNOLOGY CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LI, QINGHUA, LI, XIAOYU, LIU, HONGYU, PANG, Jing, YANG, DONG
Publication of US20210198761A1 publication Critical patent/US20210198761A1/en
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    • 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
    • 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
    • C21D6/008—Heat treatment of ferrous alloys containing Si
    • 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
    • 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
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/03—Amorphous or microcrystalline structure
    • 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

Definitions

  • the present invention relates to the field of soft magnetic material, specifically to an iron-based amorphous alloy and method for preparing the same.
  • Iron-based amorphous strip is a new energy-saving material prepared by rapid solidification technology which is used in transformer core. Comparing with conventional silicon steel transformer, it is pretty easy to be magnetized, therefore dramatically decreasing no-load loss of the transformer. If it is used in oil-immersed transformer, emission of harmful gases such as CO, SO, and NO x will be reduced, so it is called “green material of 21 st century”.
  • iron-based amorphous strip which has a saturation magnetic induction of about 1.56 T is widely used. Comparing with silicon steel which has a saturation magnetic induction of nearly 2.0 T, transformer made from iron-based amorphous material has disadvantage of large volume. In order to improve competitive power of iron-based amorphous material in transformer manufacturing industry, iron-based amorphous material with saturation magnetic induction above 1.6 T is in need to be developed.
  • Hitachi Metals. Ltd. disclosed a Fe—Si—B—C alloy named HB1, which has a saturation magnetic induction of 1.64 T.
  • the disclosed process conditions includes a process comprising blowing C-contained gases to control the C percentage on the surface of the strip making it difficult to control the process conditions during product production, and hard to ensure the stability of industrial production.
  • ferrophosphorous refining In preparation process, using a large amount of ferrophosphorous under normal condition will cause crystallization and embrittlement of strip and the performances after heat treatment is worse. If this kind of alloy is used in industrial production, ferrophosphorous refining must be carried out, which on one hand increases complexity of the process, on the other hand, smelting level should be optimized, increasing the production difficulties.
  • the technical problem solved by the present disclosure aims to provide an iron-based amorphous alloy and method for preparing the same.
  • the iron-based amorphous alloy provided by the present disclosure has a high saturation magnetic induction, glass forming ability and low loss.
  • saturation magnetic induction of the iron-based amorphous alloy is ⁇ 1.62 T.
  • atomic percentage of Si is 5.5 ⁇ b ⁇ 9.0.
  • atomic percentage of P is 0.001 ⁇ d ⁇ 0.2.
  • atomic percentage of P is 0.01 ⁇ d ⁇ 0.1.
  • the iron-based amorphous alloy 81.7 ⁇ a ⁇ 81.99, 3.0 ⁇ b ⁇ 8.0, 10.0 ⁇ c ⁇ 15.0, 0.01 ⁇ d ⁇ 0.3.
  • the present disclosure also provides method for preparing the iron-based amorphous alloy, comprising:
  • the method further comprises: performing heat treatment on the iron-based amorphous alloy strip.
  • temperature for the heat treatment is from 300 to 360° C.
  • insulation duration of the heat treatment is from 60 to 120 min
  • magnetic field strength is from 800 to 1400 A/m.
  • coercive force of the heat treated iron-based amorphous alloy strip is ⁇ 4 A/m; under condition of 50 Hz and 1.35 T, excitation power of the heat treated iron-based amorphous alloy strip is less than or equals to 0.2200 VA/kg, and core loss is ⁇ 0.1800 W/kg.
  • the iron-based amorphous alloy strip is in completely amorphous phase with a critical thickness of at least 45 ⁇ m.
  • thickness of the iron-based amorphous alloy strip is from 23 to 32 ⁇ m and width is from 100 to 300 mm.
  • the present application provides an iron-based amorphous alloy as shown in formula Fe a Si b B c P d M e , comprising Fe, Si, B and P.
  • Fe element which functions as ferromagnetic element, is the main magnetism source of iron-based amorphous alloy, ensuring high saturation magnetic induction of amorphous alloy.
  • Si and B are amorphous forming elements and an appropriate amount of which ensures good glass forming ability of the iron-based amorphous alloy.
  • P element is also amorphous forming element and an appropriate amount of P element gives amorphous alloy good glass forming ability, ensuring the magnetic properties of amorphous alloy.
  • P element can also improve the fluidity of molten alloy and reduce the pouring temperature in the preparation process, therefore reduce the difficulty of preparation. Further, in the process of iron-based amorphous alloy preparation, the present application further improves comprehensive magnetic properties of iron-based amorphous alloy by defining heating temperature and insulation duration of heat treatment and magnetic field strength.
  • FIG. 1 shows the XRD spectrum of iron-based amorphous alloy with different thicknesses of the examples and comparative examples in the present disclosure.
  • FIG. 2 shows the correlation between magnetic property and heat treatment temperature in the examples and comparative examples of the present disclosure.
  • FIG. 3 is a comparison diagram of loss curve of the examples and comparative examples in the present disclosure under condition of 50 Hz.
  • the present disclosure provides an iron-based amorphous alloy as shown in formula (I):
  • the chemical formula of the iron-based amorphous alloy is Fe a Si b B c P d M e by atomic percentage, wherein M is the unavoidable impurity element; atomic percentages of a, b, c, and d are: 80.5 ⁇ a ⁇ 84.0, 3.0 ⁇ b ⁇ 9.0, 8.0 ⁇ c ⁇ 15.0, 0.001 ⁇ d ⁇ 0.3; the rest is e: e ⁇ 0.4.
  • Fe is ferromagnetic element, which is the main magnetism source of the iron-based amorphous alloy.
  • High Fe percentage is important for ensuring high saturation magnetic induction of the iron-based amorphous alloy.
  • atomic percentage of Fe is from 80.5 to 84.0.
  • the atomic percentage of Fe is from 80.95 to 83.95; more specifically, the atomic percentage of Fe is from 81.5 to 82.5; even more specifically, the atomic percentage of Fe is 81.15, 81.35, 81.5, 81.7, 81.99, 82.05, 82.15, 82.30, 82.45, 82.65, 82.80, 82.95, 83.25, 83.55 or 83.95. If the percentage of Fe is above 83.0, the glass forming ability of alloy will decrease, making it hard to realize the industrial production.
  • the Si element and B element are amorphous forming element, which are necessary conditions for the formation of amorphous alloy system under industrial production condition.
  • the percentage of Si is from 3.0 to 9.0.
  • the percentage of Si is from 5.5 to 9.0; more specifically, the percentage of Si is 5.5, 6.0, 6.5, 6.8, 7, 7.2, 7.8, 8.0, 8.5 or 9.0.
  • the atomic percentage of Si is above 9.0, eutectic point is deviated and the glass forming ability also decreases.
  • the percentage of Si is less than 3.0, the glass forming ability of the alloy is decreased and the magnetic properties of strip are influenced.
  • the percentage of B is from 8.0 to 15.0; in specific examples, the percentage of B is 13.7 ⁇ c ⁇ 14.7; in specific examples, the percentage of B is 8.0, 8.5, 9.0, 9.5, 10.0, 10.8, 11.0, 11.2, 11.8, 12.0, 12.7, 13.0, 13.6 or 14.0.
  • the atomic percentage of B is above 16.0, the alloy components deviate from the eutectic point, causing the decrease of glass forming ability of the alloy.
  • P is also an amorphous forming element.
  • adding a trace amount of P element mainly aims to improve the fluidity of molten alloy, decreasing the pouring temperature in the preparation process and reducing the preparation difficulty.
  • addition of P element is realized by adding ferrophosphorus.
  • ferrophosphorus the quality of domestic ferrophosphorus production is not high, adding it in a large amount will introduce mass amount of impurities into the molten steel, dramatically decreasing the quality of the molten steel. This not only influences the preparation success rate of the iron-based amorphous alloy strip, making it hard for the strip to form amorphous phase, but also influences the magnetic properties of the amorphous alloy strip.
  • atomic percentage of P is from 0.001 to 0.3; in specific examples, the percentage of P is from 0.001 to 0.2; further, the percentage of P is from 0.01 to 0.1.
  • M represents impurity element and the content of M is preferred as low as possible. Therefore, the present application does not limit the content of M, as long as it is ⁇ 0.4.
  • the present disclosure provides a reasonable combination of component and content of the iron-based amorphous alloy to form an iron-based amorphous alloy with high saturation magnetic induction.
  • the present disclosure also provides a method for preparing the iron-based amorphous alloy, comprising the following steps:
  • the smelting temperature is from 1300 to 1600° C., and the duration is from 80 to 1.30 min.
  • the smelted molten alloy is heated, insulated, and then subjected to single roller rapid quenching to give iron-based amorphous alloy strip.
  • the heating temperature is preferably from 1350 to 1550° C., and the insulation duration is preferably from 90 to 120 min.
  • the spraying temperature of single roller rapid quenching is from 1300 to 1450° C., and the linear velocity of cooling roller is from 20 to 30 m/s.
  • the iron-based amorphous alloy strip is obtained, which is completely amorphous, having a critical thickness of at least 45 ⁇ m and relative good toughness, which will not crack after 180 degree folding.
  • the glass forming ability (GFA) of alloy is the size of amorphous alloy that can be obtained under certain preparation conditions, the larger the size is, the heater the glass forming ability will be.
  • critical thickness is an important index to evaluate the glass forming ability. The thicker the critical thickness is, the better the glass forming ability will be.
  • the critical thickness is at least 45 ⁇ m, which gives considerable margin for industrial production of the present product and reduces the requirement for cooling devices in industrialization process.
  • Ductile-brittle is an important index in the application of amorphous strip. In the application process, the strip will be subjected to shearing. If the fragility of the strip is high, more fragments will be generated during shearing process, which will influence the modifying of iron core and the assembling of transformer.
  • the strip of the present disclosure has a good ductile-brittle, which will not crack after 180 degree folding, and will not generate fragments in the following shearing process.
  • the thickness of the iron-based amorphous alloy strip in the present application is from 23 to 32 ⁇ m, and the width of which is from 100 to 300 mm.
  • thickness of strip is one of the important factors that influence the core loss and also a main factor that determines the superiority of amorphous strip over silicon steel in respect of no-load loss.
  • the core loss of soft magnetic material is mainly from three aspects: hysteresis loss, eddy current loss and residual loss. The thickness influences the eddy current loss directly. For magnetic material, eddy current appears on magnetic domain wall, With the flow of eddy current, magnetic influx opposite to that of the external magnetic field is generated at every moment.
  • an iron-based amorphous alloy strip with a thickness of 23 to 32 ⁇ m is prepared by choosing preparation processes. At present, the width of the strips on the market is usually 142 mm, 170 mm and 213 mm. The wider the strip is, the harder it is to be prepared.
  • heat treatment is carried out after the iron-based amorphous alloy strip is prepared.
  • the temperature for the heat treatment is from 300 to 360° C.
  • the insulation duration is from 60 to 120 min
  • the magnetic field strength is from 800 to 1400 A/m.
  • heat treatment process is also a key factor that influences the magnetic property of amorphous, nano-crystalline soft magnetic material.
  • annealing treatment can eliminate the stress of amorphous magnetic material is eliminated, reduce the coercive force and improve the magnetic permeability, therefore obtaining good magnetic property.
  • the heat treatment process mainly includes three parameters: insulation temperature, insulation duration and magnetic field strength. Firstly, the insulation temperature needs to be less than crystallization temperature.
  • crystallization temperatures of all the alloys in the present disclosure are less than 500° C. in the premise of below crystallization temperature, suitable insulation temperature range is the guarantee of the excellent magnetic property of amorphous strip.
  • core loss of the strip, excitation power and insulation temperature of heat treatment have relationship as follows: with the increase of temperature, the two parameters tend to decrease firstly and then increase, That is, for the present disclosure, the properties are adverse when the insulation temperature is lower than 300° C. or above 360° C.; qualified magnetic property can be obtained between 300 and 360° C.
  • the insulation duration has a similar influence as the insulation temperature, i.e., there is a suitable duration range. Neither unduly short insulation duration nor unduly long insulation duration can obtain optimized properties.
  • suitable magnetic field strength is a necessary guarantee for the magnetization of materials.
  • the main reason for carrying out magnetic field annealing on amorphous material is that magnetic field with fixed direction and fixed strength promotes the magnetic domain of material to turn toward the field direction, reducing magnetic anisotropy of material and optimizing soft magnetic property.
  • the magnetic field strength is less than 800 A/m, the material is not completely magnetized, so that the optimal effect cannot be reached.
  • the magnetic field strength is >1400 A/m, the material is completely magnetized.
  • the magnetic property will not be better optimized with the increase of magnetic field strength; on the contrary, extremely high magnetic field strength will increase the difficulty and cost of heat treatment.
  • the iron-based amorphous strip in the present disclosure After annealing, the iron-based amorphous strip in the present disclosure has a core loss P of ⁇ 0.1800 W/kg, excitation power Pe of ⁇ 0.2200 VA/kg and coercive force He of ⁇ 4 A/m.
  • Coercive force is an important index to evaluate the property of soft magnetic materials. The smaller coercive force is, the better the soft magnetic property will be.
  • the indexes used to evaluate the magnetic property mainly include two indexes: core loss and excitation power. The smaller the two indexes are, the better the property of the follow-up core and transformer will be. Therefore, the iron-based amorphous alloy prepared in the present disclosure can be used as core material of transformer, engine and genera tor.
  • Metal raw materials were prepared in proportion to alloy formula Fe a Si b B c P d M f and smelted in medium frequency furnace (the smelting temperature was from 1300 to 1600° C. and the insulation duration was from 80 to 130 min). After smelting, steel liquid was output to intermediate frequency furnace, heated, insulated, and stood (heated to 1350 to 1550° C. and the insulation duration was 90 to 120 min). Thereafter, single roller rapid quenching method (spray temperature was from 1300 to 1450° C. and the linear velocity of cooling roller is from 20 to 30 m/s) was used to prepare an iron-based amorphous wide strip with width of 142 mm and thickness of 23 to 28 ⁇ m. Table 1 showed alloy components, pouring temperature and critical thickness of the examples and comparative examples of the present disclosure. Therein, examples 1 to 29 were the examples of the present disclosure and examples 30 to 35 were comparative examples.
  • FIG. 1 is the XRD spectrum of iron-based amorphous alloy of the examples and comparative examples of the present disclosure. It can also be seen in conjunction with FIG. 1 and Table 1 that crystallization occurs if unduly amount of P element is added. This is mainly because the impurity percentage of industrial prepared ferrophosphorus is unduly high, so that the present disclosure cannot obtain complete amorphous strip in practical industrial production.
  • Table 2 showed saturation magnetic induction (Bs), excitation power (Pe) and core loss (P) of heat treated examples and comparative examples of the present disclosure.
  • the temperature for heat treatment was from 300 to 360° C.
  • the duration was from 60 to 120 min
  • the magnetic field strength was from 800 to 1400 A/m.
  • annular samples were used in heat treatment process: the inner diameter was 50.5 mm, the outer diameter was from 52.5 to 54.5 mm, and the testing condition was 1.35 T/50 Hz.
  • the iron-based amorphous alloy of the present disclosure have a good saturation magnetic induction, the value of which is not less than 1.62 T, higher than the conventional iron-based amorphous material used in power transformer at present, which has a saturation magnetic induction of 1.56 T (comparative example 30). Improving of saturation magnetic induction of core material makes the design of core of transformer optimized, reducing volume of the transformer and decreasing the cost. Table 2 also indicates that alloy with a components conforming to the present disclosure has good magnetic properties. Under condition of 50 Hz and 1.35 T, heat treated core has excitation power of ⁇ 0.2200 VA/kg and core loss of ⁇ 0.1800 W/kg, which meets operational requirements compared with conventional amorphous material (comparative example 31).
  • FIG. 2 shows the relationship between magnetic property and heat treatment temperature of the typical examples and comparative examples in the present disclosure.
  • ⁇ curve shows the relationship between excitation power and heat treatment temperature of Example 9; ⁇ curve shows the relationship between excitation power and heat treatment temperature of Example 20; ⁇ curve shows the relationship between excitation power and heat treatment temperature of Example 28; ⁇ curve shows the relationship between excitation power and heat treatment temperature of Comparative Example 30.
  • ⁇ curve shows the relationship between core loss and heat treatment temperature of Example 9; ⁇ curve shows the relationship between core loss and heat treatment temperature of Example 20; ⁇ curve shows the relationship between core loss and heat treatment temperature of Example 28; ⁇ curve shows the relationship between core loss and heat treatment temperature of Comparative Example 30.
  • alloy in the present disclosure has stable magnetic properties in a relative wide temperature range, at least 20° C., that is, fluctuation of excitation power (Pe) and core loss (P) is in the range of ⁇ 0.01.
  • the optimized temperature for heat treatment decreases at least 20° C., which can decrease the temperature-control requirement to heat treatment device, prolong service life of heat treatment device, and decrease the cost of heat treatment indirectly.
  • FIG. 3 is comparison diagram of loss curve of the typical examples and comparative examples in the present disclosure under condition of 50 Hz.
  • ⁇ curve is the loss curve of Example 9;
  • ⁇ curve is the loss curve of Example 20;
  • ⁇ curve is the loss curve of Example 28;
  • ⁇ curve is the loss curve of Comparative Example 30.
  • FIG. 3 demonstrates that the alloy of the present disclosure has better properties comparing with conventional iron-based amorphous alloy under working condition of relative high flux density. That is, the core and transformer made from the iron-based amorphous material prepared by the alloy components of the present disclosure can operate under working condition of higher flux density.

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CN113546653A (zh) * 2021-07-23 2021-10-26 合肥工业大学 一种用于高效降解染料的Fe-Si-B-P系非晶合金催化剂及其制备方法与应用
CN114058810A (zh) * 2021-11-18 2022-02-18 安徽中环晶研新材料有限公司 一种高性能铁基非晶纳米晶合金的热处理方法
CN115161579A (zh) * 2021-09-08 2022-10-11 武汉苏泊尔炊具有限公司 炊具及其制造方法

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CN115161579A (zh) * 2021-09-08 2022-10-11 武汉苏泊尔炊具有限公司 炊具及其制造方法
CN114058810A (zh) * 2021-11-18 2022-02-18 安徽中环晶研新材料有限公司 一种高性能铁基非晶纳米晶合金的热处理方法

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