CN102543348A - Iron-based nanocrystalline magnetically soft alloy and preparation method thereof - Google Patents
Iron-based nanocrystalline magnetically soft alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an iron-based nanocrystalline magnetically soft alloy and a preparation method thereof. The alloy is FeaCubAlcSixByPz, wherein a is more than or equal to 68 and less than or equal to 85, b is more than or equal to 0 and less than or equal to 2, c is more than or equal to 0 and less than or equal to 5, x is more than or equal to 3 and less than or equal to 18, y is more than or equal to 5 and less than or equal to 20, z is more than or equal to 0 and less than or equal to 10, and the sum of a, b, c, x, y and z is equal to 100. Compared with the prior art, the iron-based nanocrystalline magnetically soft alloy has the advantages of high saturation induction density, low loss and the like.
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 have good comprehensive soft magnet performance with nano-crystal soft magnetic alloy; Like characteristics such as the saturated magnetic strength value of height, high permeability, low-coercivity, low-loss, low exciting curent and good stable property; Iron core, filter reactor, saturable reactor, motor stator and the Magnetic Sensor etc. that can be used for distribution transformer, intermediate frequency power supply transformer and switching mode power supply transformer are to use 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; High magnetic permeability and this two big characteristic of low-loss of utilizing alloy to possess; Iron-based amorphous and nanocrystalline soft magnetic alloy can also be as the core material of novel motor stator; Be used for improving the efficient of motor, thereby reduce power consumption.This potential application is just obtaining international extensive concern at present.Investigation shows that in electricity consumption in Japan, the ratio of motor accounts for 51%.If improve the efficient of motor,, satisfy global energy-conservation requirement just can reduce the consumption of electric power.Along with the development of automobile industry, adopt the position of motor to be tending towards increasing from now on, such as electric oil pump, electric boosted steering wheel, dynamo-electric brake etc.Use novel amorphous iron core motor, can make motor miniaturization more, high efficiency, and practice thrift the consumption of rare metal (Nd), reduce the cost of motor.In addition, the 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 can be used for traffic control, wagon flow detection of intelligent transportation etc.; In intelligent grid, Magnetic Sensor can be applicable to many aspects such as the isoparametric monitoring of voltage, electric current, power and AC frequency conversion speed regulator, inverter, rectifier, communication power supply, signal monitoring, the fault location detection of electric power system.
Because the application of Fe-based amorphous nanocrystalline alloy has great economic implications and social benefit, recent decades, the research of relevant amorphous and nanometer crystal alloy was the research focus in material and the Condensed Matter Physics field all the time.The Fe-Cu-Nb-Si-B that the most noticeable research starts from people such as the Yoshizawa discovery of Hitachi Metals company in 1988 is an alloy.Because this series alloy has unique nanocrystalline structure and excellent soft magnet performance, caused that researcher's wide sending out noted.Through the research of two more than ten years, present nano-crystal soft magnetic alloy mainly comprises three alloy systems, and FeCuMSiB (M=Nb; Ta, W etc.) be Finemet alloy, FeMBCu (M=Zr, Hf; Nb etc.) be that Nanoperm alloy and FeCoMCuB (M=Zr, Hf, Nb etc.) are the Hitperm alloy.Wherein, Though Nanoperm and Hitperm alloy saturation magnetization are higher; But the soft magnetism combination property also causes cost height and complicated process of preparation because contain a large amount of precious metal elements (like Zr, Nb, Co etc.) that are prone to oxidation simultaneously not as good as the Finemet alloy, does not obtain real applying.Comprehensively soft magnet performance and lower cost are widely used the Finemet alloy at present in a lot of fields preferably owing to it.Yet its saturation induction density relatively low (the highest 1.4T that is merely is usually about 1.2T).This causes it to compare with the silicon steel of high saturated magnetic induction, needs bigger volume when under identical condition of work, using, and limits its application greatly.Be to adapt to the lightweight of device, the requirement of miniaturization development, increasing for the demand of the soft magnetic material of novel high saturated magnetic induction, high magnetic permeability, low-loss, good high frequency performance.This shows, develop a kind of have than high saturated magnetic induction and low-loss iron-based amorphous and nanocrystalline soft magnetic alloy material have great importance for the development that promotes China's iron based amorphous nanocrystalline soft magnetic material and device related industry thereof.
Summary of the invention
The object of the invention is exactly for the defective that overcomes above-mentioned prior art existence a kind of have high saturated magnetic induction and low-loss Fe-based nanocrystalline magnetically soft alloy and preparation method thereof to be provided.
The object of the invention can be realized through following technical scheme: a kind of Fe-based nanocrystalline magnetically soft alloy is characterized in that this alloy is Fe
aCu
bAl
cSi
xB
yP
z, 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.
A kind of preparation method of Fe-based nanocrystalline magnetically soft alloy is characterized in that, this method may further comprise the steps:
(1) ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminum feedstock are made into Fe according to certain ratio
aCu
bAl
cSi
xB
yP
z, the raw material that proportioning is good is packed in the crucible of vacuum medium frequency induction furnace, and the method that under vacuum condition, adopts the Medium frequency induction melting makes raw material melt back multipass alloying component even, and pours into alloy pig;
(2) alloy pig that melting is obtained is broken, and the block alloy of fragmentation is put into acetone soln successively with alcoholic solution carries out ultrasonic cleaning, take out then dry naturally for use;
(3) block alloy that cleans up is put into the quartz ampoule of chilling system carrying device, used single roller to get rid of the band method and prepare width at the 2-20 millimeter, the amorphous alloy ribbon of thickness 24-30 micron;
(4) amorphous thin ribbon that makes is put into heat-treatment furnace; Under the environment of vacuum or inert gas shielding; Heating rate with less than 20 ℃/minute is increased to 360 ℃～460 ℃ with temperature; Be incubated 30 minutes to 2 hours, cool to room temperature then with the furnace, obtain the compound iron-base soft magnetic alloy material of amorphous and nanocrystalline two-phase.
The described melting number of times of step (1) is greater than 3 times.
The system tape speed that the described single roller of step (3) gets rid of the band method is 35m/s in air.
The pressure of the described vacuum of step (4) is less than 10
-3Pa, described inert gas are argon gas.
Compared with prior art; The present invention is a raw material with ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium etc.; Handle through alloy melting, chilling system band and nanocrystalline crystallization; Make the iron-based amorphous and nanocrystalline soft magnetic alloy material, solve the lower problem of present iron-based amorphous and nanocrystalline soft magnetic alloy material saturation induction density, a kind of have high saturated magnetic induction and low-loss iron-based amorphous and nanocrystalline soft magnetic alloy material and preparation method thereof are provided.
Embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
Embodiment 1:
Is Fe with raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium according to certain proportional arrangement composition
82Cu
0.5Al
1Si
4.5B
8P
4Masterbatch, amount to 5 kilograms; With melting in the crucible of the masterbatch adding vacuum medium frequency induction furnace that configures, the Medium frequency induction melting obtains the uniform alloy pig of composition for 3 times; The alloy pig Mechanical Crushing is put into the quartz ampoule of chilling system carrying device, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making bandwidth is that 10mm, thickness are 30 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tubular type vacuum heat treatment furnace, and vacuum degree is 10
-3About Pa, be warming up to 360 ℃, be warming up to 400 ℃ with 5 ℃/minute then, and be incubated 20 minutes, cool to room temperature then with the furnace with 15 ℃/minute the rates of heat addition.The magnetic measurement that passes through of the nanocrystalline strip after the heat treatment obtains its saturation magnetization and is about 1.82T, and coercive force is about 18A/m, iron loss P
1/50=0.4W/kg.
Embodiment 2:
Is Fe with raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium according to certain proportional arrangement composition
80Cu
0.5Al
1.5Si
5B
9P
4Masterbatch, amount to 5 kilograms; With melting in the crucible of the masterbatch adding vacuum medium frequency induction furnace that configures, the Medium frequency induction melting obtains the uniform alloy pig of composition for 3 times; The alloy pig Mechanical Crushing is put into the quartz ampoule of chilling system carrying device, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making bandwidth is that 10mm, thickness are 30 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tubular type vacuum heat treatment furnace, and vacuum degree is 10
-3About Pa, be warming up to 360 ℃, be warming up to 400 ℃ with 5 ℃/minute then, and be incubated 20 minutes, cool to room temperature then with the furnace with 15 ℃/minute the rates of heat addition.The magnetic measurement that passes through of the nanocrystalline strip after the heat treatment obtains its saturation magnetization and is about 1.74T, and coercive force is about 10A/m, iron loss P
1/50=0.3W/kg.
Embodiment 3:
Is Fe with raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium according to certain proportional arrangement composition
78.5Cu
0.5Al
2Si
5.5B
9.5P
4Masterbatch, amount to 5 kilograms; With melting in the crucible of the masterbatch adding vacuum medium frequency induction furnace that configures, the Medium frequency induction melting obtains the uniform alloy pig of composition for 3 times; The alloy pig Mechanical Crushing is put into the quartz ampoule of chilling system carrying device, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making bandwidth is that 10mm, thickness are 30 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tubular type vacuum heat treatment furnace, and vacuum degree is 10
-3About Pa, be warming up to 360 ℃, be warming up to 400 ℃ with 5 ℃/minute then, and be incubated 20 minutes, cool to room temperature then with the furnace with 15 ℃/minute the rates of heat addition.The magnetic measurement that passes through of the nanocrystalline strip after the heat treatment obtains its saturation magnetization and is about 1.62T, and coercive force is about 8A/m, iron loss P
1/50=0.26W/kg.
Embodiment 4:
Is Fe with raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium according to certain proportional arrangement composition
85Cu
0Al
0Si
3B
5P
7Masterbatch, amount to 5 kilograms; With melting in the crucible of the masterbatch adding vacuum medium frequency induction furnace that configures, the Medium frequency induction melting obtains the uniform alloy pig of composition for 4 times; The alloy pig Mechanical Crushing is put into the quartz ampoule of chilling system carrying device, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making bandwidth is that 2mm, thickness are 24 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tubular type vacuum heat treatment furnace, and vacuum degree is 10
-3About Pa, be warming up to 360 ℃, be warming up to 460 ℃ with 5 ℃/minute then, and be incubated 20 minutes, cool to room temperature then with the furnace with 15 ℃/minute the rates of heat addition.The magnetic measurement that passes through of the nanocrystalline strip after the heat treatment obtains its saturation magnetization and is about 1.62T, and coercive force is about 8A/m, iron loss P
1/50=0.26W/kg.
Embodiment 5:
Is Fe with raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium according to certain proportional arrangement composition
68Cu
0Al
0Si
17B
5P
10Masterbatch, amount to 5 kilograms; With melting in the crucible of the masterbatch adding vacuum medium frequency induction furnace that configures, the Medium frequency induction melting obtains the uniform alloy pig of composition for 4 times; The alloy pig Mechanical Crushing is put into the quartz ampoule of chilling system carrying device, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making bandwidth is that 20mm, thickness are 25 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tubular type vacuum heat treatment furnace, and vacuum degree is 10
-3About Pa, be warming up to 360 ℃, be warming up to 460 ℃ with 5 ℃/minute then, and be incubated 20 minutes, cool to room temperature then with the furnace with 15 ℃/minute the rates of heat addition.The magnetic measurement that passes through of the nanocrystalline strip after the heat treatment obtains its saturation magnetization and is about 1.62T, and coercive force is about 8A/m, iron loss P
1/50=0.26W/kg.
Embodiment 6:
Is Fe with raw materials such as ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminium according to certain proportional arrangement composition
70Cu
2Al
3Si
3B
20P
0Masterbatch, amount to 5 kilograms; With melting in the crucible of the masterbatch adding vacuum medium frequency induction furnace that configures, the Medium frequency induction melting obtains the uniform alloy pig of composition for 4 times; The alloy pig Mechanical Crushing is put into the quartz ampoule of chilling system carrying device, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making bandwidth is that 15mm, thickness are 25 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tubular type vacuum heat treatment furnace, and vacuum degree is 10
-3About Pa, be warming up to 360 ℃, be warming up to 460 ℃ with 5 ℃/minute then, and be incubated 20 minutes, cool to room temperature then with the furnace with 15 ℃/minute the rates of heat addition.The magnetic measurement that passes through of the nanocrystalline strip after the heat treatment obtains its saturation magnetization and is about 1.62T, and coercive force is about 8A/m, iron loss P
1/50=0.26W/kg.
Claims (5)
1. a Fe-based nanocrystalline magnetically soft alloy is characterized in that, this alloy is Fe
aCu
bAl
cSi
xB
yP
z, 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.
2. the preparation method of a Fe-based nanocrystalline magnetically soft alloy according to claim 1 is characterized in that, this method may further comprise the steps:
(1) ferrosilicon, ferro-boron, ferrophosphorus, iron, copper, aluminum feedstock are made into Fe according to certain ratio
aCu
bAl
cSi
xB
yP
z, the raw material that proportioning is good is packed in the crucible of vacuum medium frequency induction furnace, and the method that under vacuum condition, adopts the Medium frequency induction melting makes raw material melt back multipass alloying component even, and pours into alloy pig;
(2) alloy pig that melting is obtained is broken, and the block alloy of fragmentation is put into acetone soln successively with alcoholic solution carries out ultrasonic cleaning, take out then dry naturally for use;
(3) block alloy that cleans up is put into the quartz ampoule of chilling system carrying device, used single roller to get rid of the band method and prepare width at the 2-20 millimeter, the amorphous alloy ribbon of thickness 24-30 micron;
(4) amorphous thin ribbon that makes is put into heat-treatment furnace; Under the environment of vacuum or inert gas shielding; Heating rate with less than 20 ℃/minute is increased to 360 ℃～460 ℃ with temperature; Be incubated 30 minutes to 2 hours, cool to room temperature then with the furnace, obtain the compound iron-base soft magnetic alloy material of amorphous and nanocrystalline two-phase.
3. the preparation method of Fe-based nanocrystalline magnetically soft alloy according to claim 2 is characterized in that, the described melting number of times of step (1) is greater than 3 times.
4. the preparation method of Fe-based nanocrystalline magnetically soft alloy according to claim 2 is characterized in that, the system tape speed that the described single roller of step (3) gets rid of the band method is 35m/s in air.
5. the preparation method of Fe-based nanocrystalline magnetically soft alloy according to claim 2 is characterized in that, the pressure of the described vacuum of step (4) is less than 10
-3Pa, described inert gas are argon gas.
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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 |
| CN102962465A (en) * | 2012-11-22 | 2013-03-13 | 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 |
| CN103915231A (en) * | 2014-03-03 | 2014-07-09 | 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 |
| CN106834930A (en) * | 2017-03-08 | 2017-06-13 | 中国科学院宁波材料技术与工程研究所 | The method that the alloy is prepared with the compatible iron-base nanometer crystal alloy of high magnetic flux density impurity high and using the raw material of industry |
| CN107354405A (en) * | 2017-07-31 | 2017-11-17 | 芜湖君华材料有限公司 | A kind of inexpensive iron-based amorphous alloy ribbon material production technology |
| WO2019024285A1 (en) * | 2017-07-31 | 2019-02-07 | 青岛云路先进材料技术有限公司 | Iron-based amorphous alloy |
| WO2019119637A1 (en) * | 2017-12-21 | 2019-06-27 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous alloy and preparation method therefor |
| 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 |
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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 |
| CN102962465A (en) * | 2012-11-22 | 2013-03-13 | 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 |
| CN103915231A (en) * | 2014-03-03 | 2014-07-09 | 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 |
| CN106834930A (en) * | 2017-03-08 | 2017-06-13 | 中国科学院宁波材料技术与工程研究所 | The method that the alloy is prepared with the compatible iron-base nanometer crystal alloy of high magnetic flux density impurity high and using the raw material of industry |
| CN107354405A (en) * | 2017-07-31 | 2017-11-17 | 芜湖君华材料有限公司 | A kind of inexpensive iron-based amorphous alloy ribbon material production technology |
| WO2019024285A1 (en) * | 2017-07-31 | 2019-02-07 | 青岛云路先进材料技术有限公司 | Iron-based amorphous alloy |
| WO2019119637A1 (en) * | 2017-12-21 | 2019-06-27 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous alloy and preparation method therefor |
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| 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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