CN108559926B - A kind of preparation method of Fe-based amorphous band and preparation method thereof and high frequency high magnetic permeability nanometer crystal alloy - Google Patents
A kind of preparation method of Fe-based amorphous band and preparation method thereof and high frequency high magnetic permeability nanometer crystal alloy Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/003—Making ferrous alloys making amorphous alloys
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- 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
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Abstract
The present invention provides a kind of Fe-based amorphous bands, based on molfraction, including following components: 67~74.2 parts of Fe, 16~19.2 parts of Si, 6.5~8.5 parts of B, 2.0~3.0 parts of Nb, 0.2~1 part of V, 1.0~1.3 parts of Cu and 0.1~2.2 part of Co.Fe-based amorphous band provided by the invention, containing higher silicon, so that alloy help to obtain high magnetic permeability；And the residual magnetic flux density Br of alloy after twin-stage subsequent annealing is advantageously reduced in conjunction with V and Co in limited component containing lower boron, and then improves Effective permeability of the alloy under the high frequency of 100KHz.Fe-based amorphous band provided by the invention is not necessarily to combine transverse magnetic field condition, it is only necessary to can be obtained nanocrystalline structure using twin-stage subsequent annealing, have high frequency high magnetic permeability with the alloy that this is obtained.
Description
Technical field
The invention belongs to technical field of magnetic materials more particularly to a kind of Fe-based amorphous band and preparation method thereof and high frequencies
The preparation method of high magnetic permeability nanometer crystal alloy.
Background technique
Iron-base nanometer crystal alloy is that have high magnetic permeability and low damage by one kind obtained from subsequent annealing as amorphous alloy
The novel magnetically soft alloy of consumption.Conventional iron-base nanometer crystal alloy magnetic core is by typical national standard ingredient Fe73.5Si13.5B9Nb3Cu1
Amorphous alloy ribbon is after being wound into magnetic core, then obtained from optimizing annealing process, effective magnetic under 1KHz frequency
Conductance can achieve 100,000 or so.
With the development of modern industry, it is desirable to which soft magnetic materials, such as 10KHz to 100KHz, has within the scope of higher frequency
Higher magnetic conductivity.The prior art makes full use of transverse magnetic field annealing process that the excellent of residual magnetic flux density can be effectively reduced
Gesture is annealed using vacuum transverse magnetic field, improves the magnetic conductivity under iron-base nanometer crystal alloy magnetic core high frequency condition: having under 1KHz frequency
Effect magnetic conductivity can achieve Effective permeability under 200,000 or so, 10KHz frequency and can achieve 60,000 or more, and under 100KHz frequency
Effective permeability highest can achieve 2.8 ten thousand.
But when carrying out transverse magnetic field annealing, in order to obtain biggish transverse field strength, need using 500A~800A
High current, huge energy consumption.
Also, in high frequency high permeability magnetic core preparation process, magnetic core is when carrying out transverse magnetic field annealing, due to Lorentz force
Effect, can be moved in magnetic field.Conventional solution be magnetic core is through on stainless steel rod, and with copper wire or
The metal wire of other no magnetic fixes the both ends of magnetic core, and then magnetic core is made to avoid that movement transversely or longitudinally occurs.But it deposits
The problem of in complex process, yield is small, and industrial production efficiency is low and high production cost.
Summary of the invention
In view of this, the purpose of the present invention is to provide be used to prepare the Fe-based amorphous of high frequency high magnetic permeability nanometer crystal alloy
The preparation method of band and preparation method thereof and high frequency high magnetic permeability nanometer crystal alloy, Fe-based amorphous band provided by the invention,
It is only necessary to insulation annealings, and high frequency high magnetic permeability can be obtained without the annealing of vacuum transverse magnetic field.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of Fe-based amorphous bands, based on molfraction, including following components: 67~74.2 parts
Fe, 16~19.2 parts of Si, 6.5~8.5 parts of B, 2.0~3.0 parts of Nb, 0.2~1 part of V, 1.0~1.3 parts of Cu and
0.1~2.2 part of Co.
Preferably, the Fe-based amorphous band with a thickness of 18~24 μm.
The present invention provides the preparation methods of the Fe-based amorphous band described in above-mentioned technical proposal, comprising: will include described
The master alloy that Fe-based amorphous band limits composition carries out getting rid of tape handling, obtains Fe-based amorphous band.
The present invention also provides a kind of preparation methods of high frequency high magnetic permeability nanometer crystal alloy, comprising:
(1) Fe-based amorphous band described in above-mentioned technical proposal is provided；
(2) the Fe-based amorphous band is subjected to classification subsequent annealing, obtains high frequency high magnetic permeability nanometer crystal alloy；It is described
Classification subsequent annealing under magnetic field condition without carrying out.
Preferably, the classification subsequent annealing carries out under vacuum conditions.
Preferably, the Fe-based amorphous band is successively carried out to primary subsequent annealing, heating and secondary crystallization annealing.
Preferably, the temperature of the primary subsequent annealing is 470~480 DEG C, and the time of the primary subsequent annealing is 120
~150min.
Preferably, the temperature of the secondary crystallization annealing is 530~560 DEG C, and the time of the secondary crystallization annealing is 120
~180min.
Preferably, the rate of the heating is 1~3 DEG C/min.
Preferably, before the classification subsequent annealing, further includes: the Fe-based amorphous band is wound processing, is obtained
Fe-based amorphous magnetic core；
After the Fe-based amorphous magnetic core is carried out classification subsequent annealing, obtained high frequency high magnetic permeability nanometer crystal alloy is
High frequency high magnetic permeability nanocrystalline magnet core.
The present invention provides a kind of Fe-based amorphous bands, based on molfraction, including following components: 67~74.2 parts
Fe, 16~19.2 parts of Si, 6.5~8.5 parts of B, 2.0~3.0 parts of Nb, 0.2~1 part of V, 1.0~1.3 parts of Cu and
0.1~2.2 part of Co.Fe-based amorphous band provided by the invention, the silicon containing high-content in component so that alloy have it is high
Magnetic conductivity, while there is lower Induced Anisotropy, thus can anneal without transverse magnetic field, it may have higher magnetic
Conductance；Containing the boron of lower content in alloy compositions, low residual magnetic induction is being help to obtain after twin-stage subsequent annealing
Intensity Br, while brittleness caused by silicone content height can also be reduced, increase the toughness of amorphous band.Containing certain in alloy compositions
The V and Co of amount can inhibit the phenomenon that hysteresis loop wideization caused by increasing with frequency, and then improve alloy 100KHz's
Effective permeability under high frequency.When preparing nanometer crystal alloy by annealing, Fe-based amorphous band provided by the invention is without knot
Close transverse magnetic field condition, it is only necessary to which the nanometer crystal alloy obtained using classification subsequent annealing is had under high frequency condition with higher
Imitate magnetic conductivity.Embodiment the result shows that, Fe-based amorphous band provided by the invention, it is thus only necessary to insulation annealing, without
The annealing of vacuum transverse magnetic field can be obtained under 10KHz frequency, and Effective permeability is not less than 80000；Under 100KHz frequency, effective magnetic
Conductance is up to 30000.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the XRD testing result figure of Fe-based amorphous band in the embodiment of the present invention 1；
Fig. 2 is the XRD testing result figure of Fe-based amorphous band in the embodiment of the present invention 2；
Fig. 3 is the XRD testing result figure of Fe-based amorphous band in the embodiment of the present invention 3；
Fig. 4 is the XRD testing result figure of Fe-based amorphous band in the embodiment of the present invention 4；
Fig. 5 is the XRD testing result figure of Fe-based amorphous band in the embodiment of the present invention 5.
Specific embodiment
The present invention provides a kind of Fe-based amorphous bands, based on molfraction, including following components: 67~74.2 parts
Fe, 16~19.2 parts of Si, 6.5~8.5 parts of B, 2.0~3.0 parts of Nb, 0.2~1 part of V, 1.0~1.3 parts of Cu and
0.1~2.2 part of Co.
Provided by the present invention for preparing the Fe-based amorphous band of high frequency high magnetic permeability nanometer crystal alloy, with molfraction
Meter, including 67~74.2 parts of Fe, preferably 66.5~71.5 parts, further preferably 66.8~71.0 parts, more preferably 69
~70 parts.
Based on the Fe of the molar part, Fe-based amorphous band provided by the invention is excellent including 16~19.2 parts of Si
It is selected as 16.5~19.0 parts, further preferably 17~18.8 parts, more preferably 17.5~18.5 parts, most preferably 18 parts.
Based on the Fe of the molar part, Fe-based amorphous band provided by the invention is excellent including 6.5~8.5 parts of B
It is selected as 6.6~8.0 parts, further preferably 6.65~7.5 parts, more preferably 6.7~7.0 parts, most preferably 6.8~6.9 parts.
Based on the Fe of the molar part, Fe-based amorphous band provided by the invention is excellent including 2.0~3.0 parts of Nb
It is selected as 2.1~2.4 parts, further preferably 2.15~2.35 parts, more preferably 2.2~2.3 parts.In the present invention, the iron
Contain lower boron and niobium in base amorphous band in alloy compositions, be conducive to alleviate silicone content it is higher caused by brittleness is biggish asks
Topic.
Based on the Fe of the molar part, Fe-based amorphous band provided by the invention, including 0.2~1 part of V, preferably
It is 0.3~0.8 part, further preferably 0.4~0.7 part, more preferably 0.5~0.6 part.
Based on the Fe of the molar part, Fe-based amorphous band provided by the invention is excellent including 1.0~1.3 parts of Cu
It is selected as 1.05~1.25 parts, further preferably 1.1~1.2 parts, more preferably 1.15 parts.
Based on the Fe of the molar part, Fe-based amorphous band provided by the invention is excellent including 0.1~2.2 part of Co
It is selected as 0.2~2.0 part, further preferably 0.5~1.5 part, more preferably 0.8~1.0 part.
In the present invention, the thickness of the Fe-based amorphous band is preferably 18~24 μm, and further preferably 18~22 μm,
More preferably 19~20 μm.The present invention can obtain Fe-based amorphous band of the thickness in 19~20 μ ms, this both can guarantee
Industrial high efficiency, and can guarantee that there is high Effective permeability in high frequency.
The present invention provides the preparation methods of the Fe-based amorphous band described in above-mentioned technical proposal, comprising: will include described
The master alloy that Fe-based amorphous band limits composition carries out getting rid of tape handling, obtains Fe-based amorphous band.
In the present invention, the master alloy is preferably obtained by the way of voluntarily preparing.The present invention is to the master alloy
Preparation process does not have particular/special requirement, carries out melting using mid-frequency induction heating technique well-known to those skilled in the art.At this
In invention, the preparation method of the master alloy is preferably included: will meet the metal of the Fe-based amorphous band restriction composition and ratio
It casts after raw material melting.The present invention does not have particular/special requirement to the type and dosage of the raw metal, described to be able to satisfy
The component that Fe-based amorphous band limits.
In the present invention, the melting and casting preferably carry out under air atmosphere or vacuum environment.The present invention is to described
The specific implementation form of melting and casting does not have particular/special requirement, using melting well-known to those skilled in the art and casting mode
.In an embodiment of the present invention, the melting specifically carries out in intermediate frequency furnace.
The present invention does not have particular/special requirement to the mode for getting rid of tape handling, gets rid of band using well-known to those skilled in the art
Mode.The present invention preferably melts the master alloy after obtaining molten steel, carries out getting rid of band for the molten steel using band machine is got rid of, obtain
To Fe-based amorphous band.In an embodiment of the present invention, the band machine that gets rid of is specially that pressure list roller gets rid of band machine.
The present invention is preferably 0.02~0.3MPa using spray packet pressure when band machine get rid of band is got rid of, and further preferably 0.05
~0.2MPa, more preferably 0.1~0.2MPa.The present invention is preferred using the die gap width for spraying packet when getting rid of and get rid of band with machine
For 0.3~0.5mm, further preferably 0.4mm.The present invention using get rid of copper roller linear velocity when band machine carries out getting rid of band be preferably 15~
30m/s, further preferably 20~25m/s, more preferably 20m/s.The present invention is using the temperature for getting rid of molten steel when carrying out getting rid of band with machine
Preferably 1320~1480 DEG C of degree, further preferably 1350~1450 DEG C, more preferably 1380~1400 DEG C.
The present invention provides a kind of preparation methods of high frequency high magnetic permeability nanometer crystal alloy, comprising:
(1) Fe-based amorphous band described in above-mentioned technical proposal is provided；
(2) the Fe-based amorphous band is subjected to classification subsequent annealing, obtains high frequency high magnetic permeability nanometer crystal alloy；It is described
Classification subsequent annealing under magnetic field condition without carrying out.
In the present invention, the preparation method of the Fe-based amorphous band preferably includes following steps: will include described iron-based
The master alloy that amorphous band limits composition carries out getting rid of tape handling, obtains Fe-based amorphous band.In the present invention, described Fe-based amorphous
The preparation method of band is consistent with the preparation method of Fe-based amorphous band described in above-mentioned technical proposal, and details are not described herein.
The Fe-based amorphous band is carried out classification subsequent annealing by the present invention, obtains high frequency high magnetic permeability nanometer crystal alloy.
In the present invention, the classification subsequent annealing preferably carries out under vacuum conditions, and the vacuum degree of the vacuum condition is preferably small
In 5Pa, further preferably 1~4Pa.
In the present invention, the classification subsequent annealing preferably includes: the Fe-based amorphous band is successively carried out to primary crystalline substance
Annealing, heating and secondary crystallization annealing.
In the present invention, the temperature of the primary subsequent annealing is preferably 470~480 DEG C, further preferably 472~
475℃；The time of the primary subsequent annealing is preferably 120~150min, further preferably 125~145min, more preferably
For 130~140min.In the present invention, the primary subsequent annealing makes amorphous alloy lower than crystallization temperature by inoculation(effect)
Occur in the case of degree it is partially-crystallized, to discharge a part of crystallization latent heat in advance, due to crystalline substance when weakening the annealing of subsequent secondary crystallization
Change band caused by latent heat treatment from warming phenomenon.
After completing the primary subsequent annealing, the alloy after the primary subsequent annealing is preferably warming up to second level by the present invention
After subsequent annealing temperature, secondary crystallization annealing is carried out.In the present invention, the rate of the heating is preferably 1~3 DEG C/min, into
One step is preferably 1.5~2 DEG C/min.In the present invention, the temperature of the secondary crystallization annealing is preferably 530~560 DEG C, into one
Preferably 535~555 DEG C, more preferably 540~550 DEG C of step；The time of secondary crystallization annealing is preferably 120~
180min, further preferably 125~175min, more preferably 130~160min, most preferably 150min.
In the present invention, the secondary crystallization annealing makes amorphous alloy that the two-phase knot that crystallization becomes amorphous plus nano crystalline substance occur
Structure, to have high magnetic permeability characteristic.
In the present invention, when needing to prepare high frequency high magnetic permeability nanocrystalline magnet core, before the classification subsequent annealing, preferably
Further include: the Fe-based amorphous band is wound processing, obtains Fe-based amorphous magnetic core；By the Fe-based amorphous magnetic core according to
After the classification crystallization degenerate version that above-mentioned technical proposal limits carries out classification subsequent annealing, obtained high frequency high magnetic permeability is nanocrystalline
Alloy is high frequency high magnetic permeability nanocrystalline magnet core.The present invention does not have particular/special requirement to the winding processing mode, using ability
Magnetic core winding method known to field technique personnel.The present invention is to the size of the obtained Fe-based amorphous magnetic core without spy
It is different to require, using magnetic core size well-known to those skilled in the art.In an embodiment of the present invention, the magnetic core is specific
For outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm.
After completing the classification subsequent annealing, the present invention preferably cools down the alloy after the classification subsequent annealing,
Obtain high frequency high magnetic permeability nanometer crystal alloy.The present invention does not have particular/special requirement to the mode of the cooling, using art technology
The type of cooling known to personnel.In the present invention, the alloy temperature after cooling is preferably 300 DEG C or less.
The present invention provides a kind of Fe-based amorphous bands for being used to prepare high frequency high magnetic permeability nanometer crystal alloy, by molar part
Number meter, including following components: 67~74.2 parts of Fe, 16~19.2 parts of Si, 6.5~8.5 parts of B, 2.0~3.0 parts of Nb,
0.2~1 part of V, 1.0~1.3 parts of Cu and 0.1~2.2 part of Co.
It is wound to obtain after magnetic core after twin-stage subsequent annealing using Fe-based amorphous amorphous band provided by the invention, is significantly mentioned
Height is in the Effective permeability under high frequency condition: under 10KHz frequency, Effective permeability is not less than 80000；Under 100KHz frequency, have
It imitates magnetic conductivity and is not less than 30000.
The inductance of magnetic core is directly proportional to Effective permeability, for inductance manufacturing enterprise, the higher effective magnetic conductance of use
The amorphous band of rate can be effectively reduced magnetic core weight, reduce copper wire dosage, reduce production cost, and help to obtain
, inductance value higher inductance smaller to volume, may advantageously facilitate the high frequency, high efficiency and miniaturization of electronics and electrical equipment industry.
Fe-based amorphous band provided by the invention does not need to carry out the annealing of vacuum transverse magnetic, it is thus only necessary to insulation annealing, i.e.,
High frequency high permeability magnetic core, simple process can be obtained, and it is low to consume energy, compares vacuum transverse magnetic field method for annealing, magnetic core per ton
At least reduce by 5,000 yuan of process costs.
Fe-based amorphous band provided by the invention and preparation method thereof and high frequency high magnetic permeability are received below with reference to embodiment
The preparation method of rice peritectic alloy is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16~18%), ferro-niobium (niobium content 64-66%), vanadium iron (vanadium content 50
~55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including described
Fe-based amorphous band limits the master alloy of component, wherein the molfraction of each metallic element is respectively as follows: 69.5 parts of iron, silicon 16.5
Part, 8.5 parts of boron, 3.0 parts of niobium, 1.0 parts of vanadium, 1.3 parts of copper and 0.2 part of cobalt, i.e. master alloy group is divided into Fe69.5Si16.5B8.5Nb3.0V1. 0Cu1.3Co0.2。
After master alloy is melted, band machine is got rid of using pressure list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1320 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
69.5 parts, 16.5 parts of silicon, 8.5 parts of boron, 3.0 parts of niobium, 1.0 parts of vanadium, 1.3 parts of copper and 0.2 part of cobalt, i.e., the alloy of Fe-based amorphous band
Group is divided into Fe69.5Si16.5B8.5Nb3.0V1.0Cu1.3Co0.2。
The Fe-based amorphous band being prepared with a thickness of 19 ± 1 μm, the lamination coefficient of amorphous band is 0.82, and to system
Standby obtained Fe-based amorphous band has carried out XRD detection, as a result as shown in Figure 1.As shown in Figure 1, XRD diffracting spectrum is at 44.5 degree
It nearby is rendered as an apparent broad peak, shows that the structure of band is amorphous state.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 480 DEG C, and 550 DEG C of heat preservations 120 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, and referred to as nanometer crystal alloy goes out
High frequency high magnetic permeability nanocrystalline magnet core is obtained after furnace, thus after coming out of the stove.
Magnetism testing is carried out to the high frequency high magnetic permeability nanocrystalline magnet core being prepared: when test frequency is 10KHz, electricity
Inductance value is 75 μ H, and Effective permeability is 120,000；When test frequency is 100KHz, inductance value is 20.5 μ H, Effective permeability 3.3
Ten thousand；Coercivity H=0.45A/m under static conditions.
Embodiment 2
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16~18%), ferro-niobium (niobium content 64~66%), vanadium iron (vanadium content 50
~55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including described
Fe-based amorphous band limits the master alloy of component, wherein the molfraction of each metallic element be respectively as follows: 70.5 parts of iron, 17 parts of silicon,
7.5 parts of boron, 2.5 parts of niobium, 0.5 part of vanadium, 1.3 parts of copper and 0.8 part of cobalt, i.e. master alloy group is divided into Fe70.5Si17B7.5Nb2.5V0.5Cu1. 2Co0.8。
After master alloy is melted, band machine is got rid of using pressure list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1380 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
70.5 parts, 17 parts of silicon, 7.5 parts of boron, 2.5 parts of niobium, 0.5 part of vanadium, 1.3 parts of copper and 0.8 part of cobalt, i.e., the alloy group of Fe-based amorphous band
It is divided into Fe70.5Si17B7.5Nb2.5V0.5Cu1.2Co0.8。
The Fe-based amorphous band being prepared with a thickness of 22 ± 1 μm, the lamination coefficient of amorphous band is 0.82, same right
The Fe-based amorphous band being prepared has carried out XRD detection, as a result as shown in Figure 2.As shown in Figure 2, XRD diffracting spectrum is 44.5
Degree is nearby rendered as an apparent broad peak, shows that the structure of band is amorphous state.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 480 DEG C, and 540 DEG C of heat preservations 120 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, and referred to as nanometer crystal alloy goes out
High frequency high magnetic permeability nanocrystalline magnet core is obtained after furnace, thus after coming out of the stove.
Magnetism testing is carried out to the high frequency high magnetic permeability nanocrystalline magnet core being prepared: when test frequency is 10KHz, electricity
Inductance value is 66 μ H, and Effective permeability is 10.5 ten thousand；When test frequency is 100KHz, inductance value is 18 μ H, Effective permeability 2.9
Ten thousand；Coercivity H=0.62A/m under static conditions.
Embodiment 3
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16-18%), ferro-niobium (niobium content 64-66%), vanadium iron (vanadium content 50-
55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including the iron
Base amorphous band limit component master alloy, wherein the molfraction of each metallic element be respectively as follows: 73.2 parts of iron, 17.5 parts of silicon,
7.0 parts of boron, 2.0 parts of niobium, 0.2 part of vanadium, 1.0 parts of copper and 0.1 part of cobalt, i.e. master alloy group is divided into Fe73.2Si17.5B7.0Nb2.0V0.2
Cu1.0Co0.1。
After master alloy is melted, band machine is got rid of using pressure list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1480 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
73.2 parts, 17.5 parts of silicon, 7.0 parts of boron, 2.0 parts of niobium, 0.2 part of vanadium, 1.0 parts of copper and 0.1 part of cobalt, i.e., the alloy of Fe-based amorphous band
Group is divided into Fe73.2Si17.5B7.0Nb2.0V0.2Cu1.0Co0.1。
The Fe-based amorphous band being prepared with a thickness of 20 ± 1 μm, the lamination coefficient of amorphous band is 0.82, same right
The Fe-based amorphous band being prepared has carried out XRD detection, as a result as shown in Figure 3.From the figure 3, it may be seen that XRD diffracting spectrum is 44.5
Degree is nearby rendered as an apparent broad peak, shows that the structure of band is amorphous state.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 475 DEG C, and 550 DEG C of heat preservations 120 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, and referred to as nanometer crystal alloy goes out
High frequency high magnetic permeability nanocrystalline magnet core is obtained after furnace, thus after coming out of the stove.
Magnetism testing is carried out to the high frequency high magnetic permeability nanocrystalline magnet core being prepared: when test frequency is 10KHz, electricity
Inductance value is 62 μ H, and Effective permeability is 100,000；When test frequency is 100KHz, inductance value is 17.5 μ H, Effective permeability 2.8
Ten thousand；Coercivity H=0.86A/m under static conditions.
Embodiment 4
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16-18%), ferro-niobium (niobium content 64-66%), vanadium iron (vanadium content 50-
55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including the iron
Base amorphous band limits the master alloy of component, wherein the molfraction of each metallic element is respectively as follows: 71.7 parts of iron, 18 parts of silicon, boron
6.5 parts, 2.0 parts of niobium, 0.2 part of vanadium, 1.1 parts of copper and 0.5 part of cobalt, i.e. master alloy group is divided into Fe71.7Si18B6.5Nb2.0V0.2Cu1.1
Co0.5。
After master alloy is melted, band machine is got rid of using pressure list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1420 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
71.7 parts, 18 parts of silicon, 6.5 parts of boron, 2.0 parts of niobium, 0.2 part of vanadium, 1.1 parts of copper and 0.5 part of cobalt, i.e., the alloy group of Fe-based amorphous band
It is divided into Fe71.7Si18B6.5Nb2.0V0.2Cu1.1Co0.5。
The Fe-based amorphous band being prepared with a thickness of 19 ± 1 μm, the lamination coefficient of amorphous band is 0.82, same right
The Fe-based amorphous band being prepared has carried out XRD detection, as a result as shown in Figure 4.As shown in Figure 4, XRD diffracting spectrum is 44.5
Degree is nearby rendered as an apparent broad peak, shows that the structure of band is amorphous state.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 470 DEG C, and 540 DEG C of heat preservations 120 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, and referred to as nanometer crystal alloy goes out
High frequency high magnetic permeability nanocrystalline magnet core is obtained after furnace, thus after coming out of the stove.
Magnetism testing is carried out to the high frequency high magnetic permeability nanocrystalline magnet core being prepared: when test frequency is 10KHz, electricity
Inductance value is 69 μ H, and Effective permeability is 110,000；When test frequency is 100KHz, inductance value is 20 μ H, Effective permeability 3.2
Ten thousand；Coercivity H=0.53A/m under static conditions.
Embodiment 5
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16-18%), ferro-niobium (niobium content 64-66%), vanadium iron (vanadium content 50-
55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including the iron
Base amorphous band limits the master alloy of component, wherein the molfraction of each metallic element is respectively as follows: 67 parts of iron, 19 parts of silicon, boron 8.0
Part, 3.0 parts of niobium, 0.5 part of vanadium, 1.0 parts of copper and 1.5 parts of cobalt, i.e. master alloy group is divided into Fe67Si19B8.0Nb3.0V0.5Cu1.0Co1.5。
After master alloy is melted, band machine is got rid of using pressure list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1320 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
67 parts, 19 parts of silicon, 8.0 parts of boron, 3.0 parts of niobium, 0.5 part of vanadium, 1.0 parts of copper and 1.5 parts of cobalt, i.e., the alloy compositions of Fe-based amorphous band
For Fe67Si19B8.0Nb3.0V0.5Cu1.0Co1.5。
The Fe-based amorphous band being prepared with a thickness of 24 ± 1 μm, the lamination coefficient of amorphous band is 0.82, same right
The Fe-based amorphous band being prepared has carried out XRD detection, as a result as shown in Figure 5.As shown in Figure 5, XRD diffracting spectrum is 44.5
Degree is nearby rendered as an apparent broad peak, shows that the structure of band is amorphous state.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 470 DEG C, and 530 DEG C of heat preservations 180 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, and referred to as nanometer crystal alloy goes out
High frequency high magnetic permeability nanocrystalline magnet core is obtained after furnace, thus after coming out of the stove.
Magnetism testing is carried out to the high frequency high magnetic permeability nanocrystalline magnet core being prepared: when test frequency is 10KHz, electricity
Inductance value is 62 μ H, and Effective permeability is 100,000；When test frequency is 100KHz, inductance value is 16.8 μ H, Effective permeability 2.7
Ten thousand；Coercivity H=0.92A/m under static conditions.
Comparative example 1:
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16-18%), ferro-niobium (niobium content 64-66%), vanadium iron (vanadium content 50-
55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including the iron
Base amorphous band limit component master alloy, wherein the molfraction of each metallic element be respectively as follows: 73.5 parts of iron, 15.5 parts of silicon,
7 parts of boron, 3 parts of niobium and 1.0 parts of copper, i.e. master alloy group is divided into Fe73.5Si15.5B7Nb3Cu1。
After master alloy is melted, band machine is got rid of using pressure list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1420 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
73.5 parts, 15.5 parts of silicon, 7 parts of boron, 3 parts of niobium and 1.0 parts of copper, i.e. master alloy group is divided into Fe73.5Si15.5B7Nb3Cu1。
The Fe-based amorphous band being prepared with a thickness of 20 ± 1 μm, the lamination coefficient of amorphous band is 0.82.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 470 DEG C, and 550 DEG C of heat preservations 150 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, referred to as nanometer crystal alloy.
Carry out magnetism testing to the nanocrystalline magnet core being prepared: when test frequency is 10KHz, inductance value is 50 μ H,
Effective permeability is 80,000；When test frequency is 100KHz, inductance value is 8 μ H, and Effective permeability is 1.3 ten thousand；It is rectified under static conditions
Stupid power Hc=0.62A/m.
Comparative example 2:
Using intermediate frequency furnace, the raw metal that the Fe-based amorphous band limits component proportion will be met: electrical pure iron (>
99.9%), metallic silicon (> 99%), ferro-boron (boron content 16~18%), ferro-niobium (niobium content 64~66%), vanadium iron (vanadium content 50
~55%), fine copper (> 99.9%) and pure cobalt (> 99.9%), cast after melting under vacuum conditions, obtain including described
Fe-based amorphous band limits the master alloy of component, wherein the molfraction of each metallic element is respectively as follows: 69.5 parts of iron, silicon 16.5
Part, 8.5 parts of boron, 3.0 parts of niobium, 1.0 parts of vanadium, 1.3 parts of copper and 0.2 part of cobalt, i.e. master alloy group is divided into Fe69.5Si16.5B8.5Nb3.0V1. 0Cu1.3Co0.2。
After master alloy is melted, band machine is got rid of using gravity list roller and carries out getting rid of tape handling, the temperature of alloy solution when getting rid of band
It is 1320 DEG C.It gets rid of band and obtains Fe-based amorphous band, wherein the molfraction of each metallic element is respectively as follows: iron in Fe-based amorphous band
69.5 parts, 16.5 parts of silicon, 8.5 parts of boron, 3.0 parts of niobium, 1.0 parts of vanadium, 1.3 parts of copper and 0.2 part of cobalt, i.e., the alloy of Fe-based amorphous band
Group is divided into Fe69.5Si16.5B8.5Nb3.0V1.0Cu1.3Co0.2。
The Fe-based amorphous band being prepared with a thickness of 30 ± 1 μm, the lamination coefficient of amorphous band is 0.78.
Obtained Fe-based amorphous band is wound into outer diameter 32mm, internal diameter 20mm, the ring-shaped magnetic core of height 10mm, in vacuum
Twin-stage subsequent annealing is carried out under environment: keeping the temperature 120 minutes at 480 DEG C, and 550 DEG C of heat preservations 120 are then raised to 1 DEG C/minute of speed
Minute, it is then cooled to 200 DEG C or less and removes vacuum and come out of the stove, it will amorphous known to generation this field by above-mentioned annealing process
The nano-crystallization process of alloy, the i.e. amorphous alloy translate into amorphous/nanocrystalline double structure, referred to as nanometer crystal alloy.
Carry out magnetism testing to the nanocrystalline magnet core being prepared: when test frequency is 10KHz, inductance value is 55 μ H,
Effective permeability is 9.8 ten thousand；When test frequency is 100KHz, inductance value is 12 μ H, and Effective permeability is 2.1 ten thousand；Static conditions
Lower coercivity H=0.48A/m.
As seen from the above embodiment, Fe-based amorphous band provided by the invention, it is thus only necessary to insulation annealing, without true
Empty transverse magnetic field annealing can be obtained under 10KHz frequency, and Effective permeability is not less than 80000；Under 100KHz frequency, effective magnetic conductance
Rate is up to 30000；It is stringent to use the Fe-based amorphous band for meeting thickness requirement, it is ensured that the raising of magnetic conductivity.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (3)
1. a kind of preparation method of high frequency high magnetic permeability nanometer crystal alloy, comprising:
(1) Fe-based amorphous band is provided；
(2) the Fe-based amorphous band is subjected to classification subsequent annealing, obtains high frequency high magnetic permeability nanometer crystal alloy；
The Fe-based amorphous band, based on molfraction, including following components: 67~74.2 parts of Fe, 16.5~19.0 parts
Si, 6.5~8.5 parts of B, 2.0~3.0 parts of Nb, 0.3~0.8 part of V, 1.0~1.3 parts of Cu and 0.1~2.2 part of Co；
The Fe-based amorphous band with a thickness of 19~20 μm；
The preparation method of the Fe-based amorphous band, comprising: will include the Fe-based amorphous band limit the master alloy of composition into
Row gets rid of tape handling, obtains Fe-based amorphous band；The temperature of molten steel when getting rid of band is 1380~1400 DEG C；
The classification subsequent annealing under magnetic field condition without carrying out；
The classification subsequent annealing includes: that the Fe-based amorphous band is successively carried out to primary subsequent annealing, heating and second level crystalline substance
Annealing；
The rate of the heating is 1.5~2 DEG C/min；
The temperature of the primary subsequent annealing is 470~480 DEG C, and the time of the primary subsequent annealing is 120~150min；
The temperature of the secondary crystallization annealing is 530~560 DEG C, and the time of the secondary crystallization annealing is 120~180min.
2. preparation method according to claim 1, which is characterized in that the classification subsequent annealing under vacuum conditions into
Row.
3. preparation method according to claim 1, which is characterized in that before the classification subsequent annealing, further includes: will be described
Fe-based amorphous band is wound processing, obtains Fe-based amorphous magnetic core；
After the Fe-based amorphous magnetic core is carried out classification subsequent annealing, obtained high frequency high magnetic permeability nanometer crystal alloy is high frequency
High magnetic permeability nanocrystalline magnet core.
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| CN104485192A (en) * | 2014-12-24 | 2015-04-01 | 江苏奥玛德新材料科技有限公司 | Iron-based amorphous nano-crystal soft magnetic alloy and preparation method thereof |
| CN106086714A (en) * | 2015-04-30 | 2016-11-09 | 美特格拉斯有限公司 | The wide iron-based non-crystalline alloy of the precursor of nanometer crystal alloy |
| CN107464649A (en) * | 2017-08-03 | 2017-12-12 | 江苏奥玛德新材料科技有限公司 | A kind of magnetic core with linear hysteresis curve |
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| CN104485192A (en) * | 2014-12-24 | 2015-04-01 | 江苏奥玛德新材料科技有限公司 | Iron-based amorphous nano-crystal soft magnetic alloy and preparation method thereof |
| CN106086714A (en) * | 2015-04-30 | 2016-11-09 | 美特格拉斯有限公司 | The wide iron-based non-crystalline alloy of the precursor of nanometer crystal alloy |
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