CN102543348B - A kind of Fe-based nanocrystalline magnetically soft alloy and preparation method thereof - Google Patents
A kind of Fe-based nanocrystalline magnetically soft alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Fe-based nanocrystalline magnetically soft alloy and preparation method thereof, this alloy is FeaCubAlcSixByPz, wherein 68��a��85,0��b��2,0��c��5,3��x��18,5��y��20,0��z��10, and a+b+c+x+y+z=100. Compared with prior art, the present invention has the advantage such as high saturated magnetic induction and low-loss.
Description
Technical field
The present invention relates to a kind of alloy, especially relate to a kind of Fe-based nanocrystalline magnetically soft alloy and preparation method thereof.
Background technology
Fe-based amorphous and nano-crystal soft magnetic alloy has excellent comprehensive soft magnet performance, such as features such as high saturated magnetic strength value, high permeability, low-coercivity, low-loss, low exciting curent and good stability, can be used for distribution transformer, intermediate frequency power supply transformator and the iron core of switching mode power supply transformer, filter reactor, saturable reactor, motor stator and Magnetic Sensor etc., be apply and study one of the widest amorphous nano peritectic alloy. Except the field that this Fe-based amorphous alloy of amorphous transformer is widely applied, utilize high magnetic permeability and this two big characteristic of low-loss that alloy possesses, iron-based amorphous and nanocrystalline soft magnetic alloy is also used as the core material of novel motor stator, it is used for improving the efficiency of motor, thus reducing power consumption. This potential application currently obtains international extensive concern. Investigation display, in electricity consumption in Japan, the ratio of motor accounts for 51%. If improving the efficiency of motor, just can reduce the consumption of electric power, meeting global power conservation requirement. Along with the development of automobile industry, the position of motor will be adopted to tend to increasing from now on, such as electric oil pump, electric boosted steering wheel, dynamo-electric brake etc. Use novel amorphous iron core motor, it is possible to make motor miniaturization more, high efficiency, and save the consumption of rare metal (Nd), reduce the cost of motor. Additionally, iron-based amorphous nanometer crystalline material also can be applied in many fields such as Aero-Space, automobile, industry, consumption, Internet of Things, intelligent grid as Magnetic Sensor. In Internet of Things, Magnetic Sensor may be used in the traffic control of intelligent transportation, vehicle flux monitor etc.; In intelligent grid, Magnetic Sensor can be applicable to many aspects such as the voltage of power system, electric current, the isoparametric monitoring of power and AC frequency conversion speed regulator, inverter, commutator, communication power supply, signal monitoring, fault location detection.
Have great economic implications and social benefit due to the application of Fe-based amorphous nanocrystalline alloy, recent decades, the research about amorphous and nanometer crystal alloy was the study hotspot in material and Condensed Matter Physics field all the time. The most noticeable research starts from Yoshizawa of Hitachi Metals company in 1988 et al. Fe-Cu-Nb-Si-B system alloy found. Have the nanocrystalline structure of uniqueness and excellent soft magnet performance due to this series alloy, wide the sending out causing research worker notes. Through the research of more than 20 years, current nano-crystal soft magnetic alloy mainly includes three alloy systems, and FeCuMSiB (M=Nb, Ta, W etc.) be Finemet alloy, FeMBCu (M=Zr, Hf, Nb etc.) it is Nanoperm alloy and FeCoMCuB (M=Zr, Hf, Nb etc.) it is Hitperm alloy. Wherein, although Nanoperm and Hitperm alloy saturation magnetization is higher, but soft magnetism combination property is not as good as Finemet alloy, simultaneously also as cause cost high and complicated process of preparation containing precious metal element (such as Zr, Nb, Co etc.) oxidizable in a large number, do not obtain real popularization and application. Due to it, comprehensive soft magnet performance and relatively low cost are widely used Finemet alloy at present in a lot of fields preferably. But its saturation induction density relatively low (only up to 1.4T, generally at about 1.2T). This causes that it is compared with the silicon steel of high saturated magnetic induction, needs bigger volume, limit its application greatly under identical working condition during application. For adapting to the requirement of the lightweight of device, miniaturization, for novel high saturated magnetic induction, high magnetic permeability, low-loss, good high frequency performance the demand of soft magnetic materials increasing. As can be seen here, develop and a kind of have compared with high saturated magnetic induction and low-loss iron-based amorphous and nanocrystalline soft magnetic alloy material for promoting that the development of China's iron based amorphous nanocrystalline soft magnetic material and device related industry thereof has great importance.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide one to have high saturated magnetic induction and low-loss Fe-based nanocrystalline magnetically soft alloy and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions: a kind of Fe-based nanocrystalline magnetically soft alloy, it is characterised in that this alloy is FeaCubAlcSixByPz, wherein 68��a��85,0��b��2,0��c��5,3��x��18,5��y��20,0��z��10, and a+b+c+x+y+z=100.
The preparation method of a kind of Fe-based nanocrystalline magnetically soft alloy, it is characterised in that the method comprises the following steps:
(1) ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum feedstock are made into Fe according to certain ratioaCubAlcSixByPz, raw material good for proportioning is loaded in the crucible of vacuum medium frequency induction furnace, adopts the method for Medium frequency induction melting raw material melt back multipass under vacuum, make alloying component uniform, and pour into alloy pig;
(2) alloy pig that melting obtains is crushed, broken block alloy is sequentially placed in acetone soln and alcoholic solution and carries out ultrasonic cleaning, naturally dry stand-by after taking-up;
(3) block alloy cleaned up is put in the quartz ampoule of chilling carrying device, use melt spinning to prepare width at 2-20 millimeter, the amorphous alloy ribbon of thickness 24-30 micron;
(4) prepared amorphous thin ribbon is put in heat-treatment furnace; under the environment of vacuum or inert gas shielding; with the heating rate less than 20 DEG C/min, temperature is increased to 360 DEG C��460 DEG C; it is incubated 30 minutes to 2 hours; then cool to room temperature with the furnace, obtain the iron-base soft magnetic alloy material of amorphous and Nanocrystalline Two-phase compound.
Melting number of times described in step (1) is more than 3 times.
The tape speed processed of the melt spinning described in step (3) is 35m/s in atmosphere.
The pressure of the vacuum described in step (4) is less than 10-3Pa, described noble gas is argon.
Compared with prior art, the present invention is with ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum etc. for raw material, by alloy melting, chilling band and nanocrystalline Crystallizing treatment, prepare iron-based amorphous and nanocrystalline soft magnetic alloy material, solve the problem that current iron-based amorphous and nanocrystalline soft magnetic alloy material saturation induction density is relatively low, it is provided that one has high saturated magnetic induction and low-loss iron-based amorphous and nanocrystalline soft magnetic alloy material and preparation method thereof.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
It is Fe by raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum according to certain proportional arrangement composition82Cu0.5Al1Si4.5B8P4Masterbatch, amount to 5 kilograms; The masterbatch configured adds melting in the crucible of vacuum medium frequency induction furnace, and Medium frequency induction melting obtains the uniform alloy pig of composition for 3 times; Alloy pig Mechanical Crushing being put in the quartz ampoule of chilling carrying device, adopt sensing heating and melting, utilize single roller chilling belt-rejecting technology, in atmosphere with the speed band of 35m/s, prepared bandwidth is 10mm, thickness is the amorphous thin ribbon of 30 microns; Being put into by amorphous alloy strips in tube type vacuum heat-treatment furnace, vacuum is 10-3About Pa, is warming up to 360 DEG C with the rate of heat addition of 15 DEG C/min, is then warming up to 400 DEG C with 5 DEG C/min, and is incubated 20 minutes, then cools to room temperature with the furnace. The obtaining its saturation magnetization by magnetic measurement and be about 1.82T of nanocrystalline strip after heat treatment, coercivity is about 18A/m, iron loss P1/50=0.4W/kg.
Embodiment 2:
It is Fe by raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum according to certain proportional arrangement composition80Cu0.5Al1.5Si5B9P4Masterbatch, amount to 5 kilograms; The masterbatch configured adds melting in the crucible of vacuum medium frequency induction furnace, and Medium frequency induction melting obtains the uniform alloy pig of composition for 3 times; Alloy pig Mechanical Crushing being put in the quartz ampoule of chilling carrying device, adopt sensing heating and melting, utilize single roller chilling belt-rejecting technology, in atmosphere with the speed band of 35m/s, prepared bandwidth is 10mm, thickness is the amorphous thin ribbon of 30 microns; Being put into by amorphous alloy strips in tube type vacuum heat-treatment furnace, vacuum is 10-3About Pa, is warming up to 360 DEG C with the rate of heat addition of 15 DEG C/min, is then warming up to 400 DEG C with 5 DEG C/min, and is incubated 20 minutes, then cools to room temperature with the furnace. The obtaining its saturation magnetization by magnetic measurement and be about 1.74T of nanocrystalline strip after heat treatment, coercivity is about 10A/m, iron loss P1/50=0.3W/kg.
Embodiment 3:
It is Fe by raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum according to certain proportional arrangement composition78.5Cu0.5Al2Si5.5B9.5P4Masterbatch, amount to 5 kilograms; The masterbatch configured adds melting in the crucible of vacuum medium frequency induction furnace, and Medium frequency induction melting obtains the uniform alloy pig of composition for 3 times; Alloy pig Mechanical Crushing being put in the quartz ampoule of chilling carrying device, adopt sensing heating and melting, utilize single roller chilling belt-rejecting technology, in atmosphere with the speed band of 35m/s, prepared bandwidth is 10mm, thickness is the amorphous thin ribbon of 30 microns; Being put into by amorphous alloy strips in tube type vacuum heat-treatment furnace, vacuum is 10-3About Pa, is warming up to 360 DEG C with the rate of heat addition of 15 DEG C/min, is then warming up to 400 DEG C with 5 DEG C/min, and is incubated 20 minutes, then cools to room temperature with the furnace. The obtaining its saturation magnetization by magnetic measurement and be about 1.62T of nanocrystalline strip after heat treatment, coercivity is about 8A/m, iron loss P1/50=0.26W/kg.
Embodiment 4:
It is Fe by raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum according to certain proportional arrangement composition85Cu0Al0Si3B5P7Masterbatch, amount to 5 kilograms; The masterbatch configured adds melting in the crucible of vacuum medium frequency induction furnace, and Medium frequency induction melting obtains the uniform alloy pig of composition for 4 times; Alloy pig Mechanical Crushing being put in the quartz ampoule of chilling carrying device, adopt sensing heating and melting, utilize single roller chilling belt-rejecting technology, in atmosphere with the speed band of 35m/s, prepared bandwidth is 2mm, thickness is the amorphous thin ribbon of 24 microns; Being put into by amorphous alloy strips in tube type vacuum heat-treatment furnace, vacuum is 10-3About Pa, is warming up to 360 DEG C with the rate of heat addition of 15 DEG C/min, is then warming up to 460 DEG C with 5 DEG C/min, and is incubated 20 minutes, then cools to room temperature with the furnace. The obtaining its saturation magnetization by magnetic measurement and be about 1.62T of nanocrystalline strip after heat treatment, coercivity is about 8A/m, iron loss P1/50=0.26W/kg.
Embodiment 5:
It is Fe by raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum according to certain proportional arrangement composition68Cu0Al0Si17B5P10Masterbatch, amount to 5 kilograms; The masterbatch configured adds melting in the crucible of vacuum medium frequency induction furnace, and Medium frequency induction melting obtains the uniform alloy pig of composition for 4 times; Alloy pig Mechanical Crushing being put in the quartz ampoule of chilling carrying device, adopt sensing heating and melting, utilize single roller chilling belt-rejecting technology, in atmosphere with the speed band of 35m/s, prepared bandwidth is 20mm, thickness is the amorphous thin ribbon of 25 microns; Being put into by amorphous alloy strips in tube type vacuum heat-treatment furnace, vacuum is 10-3About Pa, is warming up to 360 DEG C with the rate of heat addition of 15 DEG C/min, is then warming up to 460 DEG C with 5 DEG C/min, and is incubated 20 minutes, then cools to room temperature with the furnace. The obtaining its saturation magnetization by magnetic measurement and be about 1.62T of nanocrystalline strip after heat treatment, coercivity is about 8A/m, iron loss P1/50=0.26W/kg.
Embodiment 6:
It is Fe by raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum according to certain proportional arrangement composition70Cu2Al3Si3B20P0Masterbatch, amount to 5 kilograms; The masterbatch configured adds melting in the crucible of vacuum medium frequency induction furnace, and Medium frequency induction melting obtains the uniform alloy pig of composition for 4 times; Alloy pig Mechanical Crushing being put in the quartz ampoule of chilling carrying device, adopt sensing heating and melting, utilize single roller chilling belt-rejecting technology, in atmosphere with the speed band of 35m/s, prepared bandwidth is 15mm, thickness is the amorphous thin ribbon of 25 microns; Being put into by amorphous alloy strips in tube type vacuum heat-treatment furnace, vacuum is 10-3About Pa, is warming up to 360 DEG C with the rate of heat addition of 15 DEG C/min, is then warming up to 460 DEG C with 5 DEG C/min, and is incubated 20 minutes, then cools to room temperature with the furnace. The obtaining its saturation magnetization by magnetic measurement and be about 1.62T of nanocrystalline strip after heat treatment, coercivity is about 8A/m, iron loss P1/50=0.26W/kg.
Claims (3)
1. the preparation method of a Fe-based nanocrystalline magnetically soft alloy, it is characterised in that the method comprises the following steps:
(1) ferrosilicon, ferro-boron, ferrophosphorus, ferrum, copper, aluminum feedstock are made into Fe according to certain ratioaCubAlcSixByPzWherein 68��a��85,0��b��2,0��c��5,3��x��18,5��y��20,0��z��10, and a+b+c+x+y+z=100, raw material good for proportioning is loaded in the crucible of vacuum medium frequency induction furnace, adopt the method for Medium frequency induction melting raw material melt back multipass under vacuum, make alloying component uniform, and pour into alloy pig;
(2) alloy pig that melting obtains is crushed, broken block alloy is sequentially placed in acetone soln and alcoholic solution and carries out ultrasonic cleaning, naturally dry stand-by after taking-up;
(3) block alloy cleaned up is put in the quartz ampoule of chilling carrying device, use melt spinning to prepare width at 2-20 millimeter, the amorphous alloy ribbon of thickness 24-30 micron; The tape speed processed of described melt spinning is 35m/s in atmosphere;
(4) prepared amorphous alloy ribbon is put in heat-treatment furnace; under the environment of vacuum or inert gas shielding; with the heating rate less than 20 DEG C/min, temperature is increased to 360 DEG C��460 DEG C; it is incubated 30 minutes to 2 hours; then cool to room temperature with the furnace, obtain the iron-base soft magnetic alloy material of amorphous and Nanocrystalline Two-phase compound.
2. the preparation method of Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the melting number of times described in step (1) is more than 3 times.
3. the preparation method of Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the pressure of the vacuum described in step (4) is less than 10-3Pa, described noble gas is argon.
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| CN102732811A (en) * | 2012-06-21 | 2012-10-17 | 四川大学苏州研究院 | High-saturated magnetization intensity Fe-based amorphous nanocrystalline soft magnetic alloy and its preparation method |
| CN102962465B (en) * | 2012-11-22 | 2015-02-04 | 德清森腾电子科技有限公司 | Low-permeability, low-power consumption Fe-Si-Al soft magnetic material and production method thereof |
| CN103915231B (en) * | 2014-03-03 | 2017-01-18 | 郑州大学 | Iron-based amorphous-nanometer crystalline state magnetically soft alloy with high saturation magnetic induction density and application thereof |
| CN104831169A (en) * | 2015-04-08 | 2015-08-12 | 朗峰新材料南通有限公司 | Fe-based nano crystal soft magnetic alloy material and preparation method thereof |
| CN105978173A (en) * | 2016-06-23 | 2016-09-28 | 无锡新大力电机有限公司 | Novel material motor stator |
| CN106834930B (en) * | 2017-03-08 | 2018-10-19 | 中国科学院宁波材料技术与工程研究所 | Iron-base nanometer crystal alloy with the high impurity compatibility of high magnetic flux density and the method for preparing the alloy using the raw material of industry |
| CN107236911A (en) * | 2017-07-31 | 2017-10-10 | 青岛云路先进材料技术有限公司 | A kind of Fe-based amorphous alloy |
| CN107354405B (en) * | 2017-07-31 | 2018-12-14 | 芜湖君华材料有限公司 | A kind of low cost iron-based amorphous alloy ribbon material production technology |
| CN108018504B (en) * | 2017-12-21 | 2020-05-08 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous alloy and preparation method thereof |
| CN111101076A (en) * | 2019-12-27 | 2020-05-05 | 中国科学院宁波材料技术与工程研究所 | Iron-based nanocrystalline magnetically soft alloy |
| CN112048602A (en) * | 2020-07-28 | 2020-12-08 | 信维通信（江苏）有限公司 | High Bs nanocrystalline strip, high Bs nanocrystalline shielding piece and preparation method thereof |
| CN111910135A (en) * | 2020-08-13 | 2020-11-10 | 合肥工业大学 | Iron-based soft magnetic alloy Fe-Co-Si-B-P-Ti and preparation method thereof |
| CN113035485A (en) * | 2021-03-04 | 2021-06-25 | 深圳市麦捷微电子科技股份有限公司 | High-magnetic-flux-density low-loss iron-based nanocrystalline magnetically soft alloy and preparation method thereof |
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