CN102953020A - Fe-based amorphous nanocrystalline soft magnetic alloy material and preparation method thereof - Google Patents
Fe-based amorphous nanocrystalline soft magnetic alloy material and preparation method thereof Download PDFInfo
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- CN102953020A CN102953020A CN2012104231595A CN201210423159A CN102953020A CN 102953020 A CN102953020 A CN 102953020A CN 2012104231595 A CN2012104231595 A CN 2012104231595A CN 201210423159 A CN201210423159 A CN 201210423159A CN 102953020 A CN102953020 A CN 102953020A
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Abstract
The invention discloses a Fe-based amorphous nanocrystalline soft magnetic alloy material, which is characterized by consisting of iron, ferroboron, ferrosilicon, copper, ferrocolumbium and cobalt. Atomic percentage ratio of each component can be expressed as (Fe1-XCoX)76.5Cu1Nb2Si11.5B9, wherein X satisfies the relation of: 0.3<=X<=0.6. The preparation method of the Fe-based amorphous nanocrystalline soft magnetic alloy material provided by the invention comprises steps of: raw material proportioning, alloy smelting, quenching for preparing belt and nanocrystalline crystallization treatment. The invention has advantages of simple process, low cost and easy mass production; and the material provided by the invention has good high frequency magnetic properties.
Description
Technical field
The present invention relates to a kind of preparation method of magnetically soft alloy material, especially a kind of iron-based amorphous and nanocrystalline soft magnetic alloy material preparation method with good high frequency performance.
Background technology
Fe-based amorphous and nano-crystal soft magnetic alloy has good comprehensive soft magnetic performance, such as characteristics such as the saturated magnetic strength value of height, high permeability, low-coercivity, low-loss, low magnetizing current and satisfactory stability, can be used for iron core, filter reactor, transductor, motor stator and the Magnetic Sensor etc. of substation transformer, intermediate frequency power supply transformer and switching mode power supply transformer, is one of the widest amorphous nano peritectic alloy of application and research.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 study hotspot in material and the Condensed Matter Physics field all the time.The Fe-Cu-Nb-Si-B that the most noticeable research starts from the people such as the Yoshizawa discovery of Hitachi Metals company in 1988 is alloy.Because this series alloy has unique nanocrystalline structure and excellent soft magnetic performance, caused that researchist's wide sending out noted.Herzer utilizes random anisotropy model to explain that nanometer crystal alloy obtains the mechanism of excellent soft magnetic property.Non-crystaline amorphous metal forms the nanocrystal that is uniformly distributed in noncrystal substrate behind Annealing Crystallization, intercrystalline spin-exchange-coupled averages out magnetocrystalline anisotropy, thereby the effective anisotropy constant reduces greatly, causes nanometer crystal alloy to obtain excellent soft magnetic property.Fe base nanometer crystal non-retentive alloy is take FeNbSiBCu (trade names are as Finemet) and FeZrBCu (trade names are as Nanoperm) as Typical Representative, under low frequency condition, have high saturation induction density and magnetic permeability, the soft magnetic property that low coercive force etc. are excellent.Development along with power technology, require soft magnetic materials under higher frequency, to work, and FINEMET type alloy under high frequency because lower resonant frequency, only can under less than the 40kHz condition, use, must manage to improve its resonant frequency in order under higher frequency, to use.
Be the requirement of the high frequency development that adapts to the power electronics information apparatus, increasing for the demand of novel soft magnetic materials with good high frequency performance.This shows, develop a kind of iron-based amorphous and nanocrystalline soft magnetic alloy material with good high frequency performance and have great importance for the development that promotes China's iron based amorphous nanocrystalline soft magnetic material and device related industries thereof.
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Summary of the invention
The present invention seeks to: a kind of present iron-based amorphous and nanocrystalline soft magnetic alloy material applying frequency lower problem of solving is provided, has the iron-based amorphous and nanocrystalline soft magnetic alloy material preparation method of good high frequency performance.
Technical scheme of the present invention is:
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy material is characterized in that, described iron-based amorphous and nanocrystalline soft magnetic alloy material is comprised of iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt metal,
Wherein the proportioning of each component can be expressed as (Fe 1-X Co X ) 76.5 Cu 1 Nb 2 Si 11.5 B 9 , 0.3≤X≤0.6 wherein, proportioning is atomic percent.
Above-mentioned iron-based amorphous and nanocrystalline soft magnetic alloy material preparation method specifically comprises the following steps:
(1) material batching: iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt raw metal are configured to be divided into (Fe according to aforementioned proportion
1-X
Co
X
)
76.5
Cu
1
Nb
2
Si
11.5
B
9
Masterbatch;
(2) alloy melting: the masterbatch for preparing is packed in the crucible of vacuum melting furnace, adopt the method for Medium frequency induction melting at lower raw material melt back multipass of vacuum condition, greater than 3 times, and in fusion process, stir, make alloying constituent even, and casting ingot-forming;
The principle of the method for Medium frequency induction melting is: masterbatch is subjected to the effect of electromagnetic induction to produce induced potential, in masterbatch, form induced current (eddy current), induced current overcomes the resistance of masterbatch itself and produces joule heating, with this heat heating masterbatch itself, makes its intensification.
(3) ultrasonic cleaning: the alloy cast ingot that melting obtains is broken, the block alloy of fragmentation is put into spirituous solution successively carry out ultrasonic cleaning, naturally dry stand-by after taking out;
(4) chilling band processed: the block alloy that cleans up is put into the silica tube of chilling carrying equipment processed, and heating and melting is used melt spinning to prepare width and is 2-50mm, and thickness is the alloy thin band of 20 ~ 25 μ m;
The principle of melt spinning is: molten alloy is sprayed to the cooling roller surface of high speed rotating, form a transient equilibrium weld pool at roll surface during injection, molten alloy will fast setting, forms alloy thin band.
(5) nano-crystallization is processed: the strip that makes is put into heat treatment furnace; under the environment of vacuum (pressure is less than 10-2Pa) or inert argon gas shield; with the temperature rise rate less than 30 ℃/minute temperature is increased to 400 ℃～480 ℃; be incubated 30 minutes to 2 hours; then cool to room temperature with the furnace, obtain the compound iron-base soft magnetic alloy material of amorphous nano-crystalline two-phase.
Advantage of the present invention is:
1. technique of the present invention is simple, cost is lower, easily mass-produced;
2. material of the present invention has good high-gradient magnetism energy.
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Embodiment:
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for explanation the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment 1:
Be the masterbatch of (Fe0.7Co0.3) 76.5Cu1Nb2Si11.5B9 with iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt raw metal according to certain proportional arrangement composition, amount to 1 kilogram; The masterbatch that configures is added melting in the crucible of vacuum medium frequency induction furnace, the Medium frequency induction melting obtains the alloy pig of homogeneous chemical composition for 4 times; The alloy pig Mechanical Crushing is put into the silica tube of chilling carrying equipment processed, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed of 25m/s band processed, making bandwidth is that 10mm, thickness are 25 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tube type vacuum heat treatment furnace, and vacuum tightness is warming up to 360 ℃ with 30 ℃/minute heating rate about 10-2Pa, then be warming up to 480 ℃ with 5 ℃/minute, and be incubated 30 minutes, then cools to room temperature with the furnace.The magnetic measurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.34T, and initial permeability is 40000, and resonant frequency is 106Hz.
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Embodiment 2:
Be the masterbatch of (Fe0.6Co0.4) 76.5Cu1Nb2Si11.5B9 with iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt raw metal according to certain proportional arrangement composition, amount to 1 kilogram; The masterbatch that configures is added melting in the crucible of vacuum medium frequency induction furnace, the Medium frequency induction melting obtains the alloy pig of homogeneous chemical composition for 4 times; The alloy pig Mechanical Crushing is put into the silica tube of chilling carrying equipment processed, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed of 25m/s band processed, making bandwidth is that 20mm, thickness are 25 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tube type vacuum heat treatment furnace, and vacuum tightness is warming up to 360 ℃ with 25 ℃/minute heating rate about 10-2Pa, then be warming up to 470 ℃ with 5 ℃/minute, and be incubated 1 hour, then cools to room temperature with the furnace.The magnetic measurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.36T, and initial permeability is 35000, and resonant frequency is 1.2 * 106Hz.
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Embodiment 3:
Be the masterbatch of (Fe0.5Co0.5) 76.5Cu1Nb2Si11.5B9 with iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt raw metal according to certain proportional arrangement composition, amount to 1 kilogram; The masterbatch that configures is added melting in the crucible of vacuum medium frequency induction furnace, the Medium frequency induction melting obtains the alloy pig of homogeneous chemical composition for 4 times; The alloy pig Mechanical Crushing is put into the silica tube of chilling carrying equipment processed, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed of 30m/s band processed, making bandwidth is that 30mm, thickness are 20 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tube type vacuum heat treatment furnace, pass into argon shield, be warming up to 360 ℃ with 20 ℃/minute heating rate, then be warming up to 460 ℃ with 5 ℃/minute, and be incubated 1 hour, then cool to room temperature with the furnace.The magnetic measurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.4T, and initial permeability is 32000, and resonant frequency is 1.5 * 106Hz.
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Embodiment 4:
Be the masterbatch of (Fe0.4Co0.6) 76.5Cu1Nb2Si11.5B9 with iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt raw metal according to certain proportional arrangement composition, amount to 1 kilogram; The masterbatch that configures is added melting in the crucible of vacuum medium frequency induction furnace, the Medium frequency induction melting obtains the alloy pig of homogeneous chemical composition for 4 times; The alloy pig Mechanical Crushing is put into the silica tube of chilling carrying equipment processed, adopt induction heating to melt, utilize single roller chilling belt-rejecting technology, with the speed of 30m/s band processed, making bandwidth is that 30mm, thickness are 20 microns amorphous thin ribbon in air; Amorphous alloy strips is put into the tube type vacuum heat treatment furnace, pass into argon shield, be warming up to 360 ℃ with 15 ℃/minute heating rate, then be warming up to 450 ℃ with 5 ℃/minute, and be incubated 2 hours, then cool to room temperature with the furnace.The magnetic measurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.45T, and initial permeability is 29000, and resonant frequency is 2.1 * 106Hz.
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Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (2)
1. an iron-based amorphous and nanocrystalline soft magnetic alloy material is characterized in that, described iron-based amorphous and nanocrystalline soft magnetic alloy material is comprised of iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt metal, and wherein the proportioning of each component can be expressed as (Fe
1-XCo
X)
76.5Cu
1Nb
2Si
11.5B
9, 0.3≤X≤0.6 wherein, proportioning is atomic percent.
2. iron-based amorphous and nanocrystalline soft magnetic alloy material preparation method claimed in claim 1 is characterized in that, specifically comprises the following steps:
(1) material batching: iron, ferro-boron, ferrosilicon, copper, ferro-niobium and cobalt raw metal are configured to be divided into (Fe according to aforementioned proportion
1-XCo
X)
76.5Cu
1Nb
2Si
11.5B
9Masterbatch;
(2) alloy melting: the masterbatch for preparing is packed in the crucible of vacuum intermediate-frequency induction melting furnace, adopt the method for Medium frequency induction melting under vacuum condition, masterbatch to be heated to fusing, about 1350 ℃, be incubated 1 hour, and in fusion process, stir, make alloying constituent even, and casting ingot-forming;
(3) ultrasonic cleaning: the alloy cast ingot that melting obtains is broken, the block alloy of fragmentation is put into spirituous solution successively carry out ultrasonic cleaning, naturally dry stand-by after taking out;
(4) chilling band processed: the block alloy that cleans up is put into the silica tube of rapid solidification carrying equipment processed, and heating and melting is used melt spinning to prepare width and is 2-50mm, and thickness is the alloy thin band of 20 ~ 25 μ m;
(5) nano-crystallization is processed: the strip that makes is put into heat treatment furnace, and in vacuum, namely pressure is less than 10
-2Under the environment of Pa or inert argon gas shield; with the temperature rise rate less than 30 ℃/minute temperature is increased to 400 ℃～480 ℃; be incubated 30 minutes to 2 hours, then cool to room temperature with the furnace, obtain the compound iron-base soft magnetic alloy material of amorphous nano-crystalline two-phase.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602931A (en) * | 2013-11-07 | 2014-02-26 | 同济大学 | Iron-based amorphous nanocrystalline soft magnetic alloy and preparation method thereof |
| CN104802042A (en) * | 2015-04-24 | 2015-07-29 | 天津理工大学 | Method for improving initial permeability and alternating-current magnetic property of amorphous magnetically-soft alloy |
| CN106282621A (en) * | 2016-08-31 | 2017-01-04 | 河北创谱金属材料检测技术有限公司 | A kind of Metal Melting alloy master batch weight, the different ferroalloy gross weight of addition and addition single ferroalloy weight method for determination of amount |
| CN106334798A (en) * | 2016-09-09 | 2017-01-18 | 电子科技大学 | Preparation method for Fe-based nanocrystalline alloy flake micropowder |
| 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 |
| CN108330412A (en) * | 2018-01-29 | 2018-07-27 | 江苏知行科技有限公司 | A kind of non-crystaline amorphous metal and its production technology |
| CN109576608A (en) * | 2018-11-14 | 2019-04-05 | 江苏科技大学 | In-situ preparation containment structure iron-base block amorphous alloy composition and preparation method thereof |
| CN109801783A (en) * | 2019-02-15 | 2019-05-24 | 信维通信（江苏）有限公司 | A kind of preparation method of the amorphous antifreeze plate for wireless charging |
| CN110423957A (en) * | 2019-08-30 | 2019-11-08 | 江苏丰创新材料有限公司 | The production method of iron-based amorphous nanometer crystalline band |
| WO2020042534A1 (en) * | 2018-08-31 | 2020-03-05 | 江西大有科技有限公司 | Low-loss nanocrystalline alloy soft magnetic material and preparation method therefor |
| CN112164541A (en) * | 2020-10-15 | 2021-01-01 | 太原理工大学 | Anti-direct-current iron-based nanocrystalline alloy and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602931A (en) * | 2013-11-07 | 2014-02-26 | 同济大学 | Iron-based amorphous nanocrystalline soft magnetic alloy and preparation method thereof |
| CN104802042A (en) * | 2015-04-24 | 2015-07-29 | 天津理工大学 | Method for improving initial permeability and alternating-current magnetic property of amorphous magnetically-soft alloy |
| CN106282621A (en) * | 2016-08-31 | 2017-01-04 | 河北创谱金属材料检测技术有限公司 | A kind of Metal Melting alloy master batch weight, the different ferroalloy gross weight of addition and addition single ferroalloy weight method for determination of amount |
| CN106282621B (en) * | 2016-08-31 | 2018-04-03 | 河北创谱金属材料检测技术有限公司 | One kind adds different ferroalloy gross weights and adds single ferroalloy weight method for determination of amount |
| CN106334798B (en) * | 2016-09-09 | 2019-11-15 | 电子科技大学 | The preparation method of Fe Based Nanocrystalline Alloys sheet micro mist |
| CN106334798A (en) * | 2016-09-09 | 2017-01-18 | 电子科技大学 | Preparation method for Fe-based nanocrystalline alloy flake micropowder |
| 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 |
| CN108330412A (en) * | 2018-01-29 | 2018-07-27 | 江苏知行科技有限公司 | A kind of non-crystaline amorphous metal and its production technology |
| WO2020042534A1 (en) * | 2018-08-31 | 2020-03-05 | 江西大有科技有限公司 | Low-loss nanocrystalline alloy soft magnetic material and preparation method therefor |
| CN109576608A (en) * | 2018-11-14 | 2019-04-05 | 江苏科技大学 | In-situ preparation containment structure iron-base block amorphous alloy composition and preparation method thereof |
| CN109801783A (en) * | 2019-02-15 | 2019-05-24 | 信维通信（江苏）有限公司 | A kind of preparation method of the amorphous antifreeze plate for wireless charging |
| CN110423957A (en) * | 2019-08-30 | 2019-11-08 | 江苏丰创新材料有限公司 | The production method of iron-based amorphous nanometer crystalline band |
| CN112164541A (en) * | 2020-10-15 | 2021-01-01 | 太原理工大学 | Anti-direct-current iron-based nanocrystalline alloy and preparation method thereof |
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Application publication date: 20130306 |