CN107393671B - A kind of iron based nanocrystalline magnet core and preparation method thereof - Google Patents
A kind of iron based nanocrystalline magnet core and preparation method thereof Download PDFInfo
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- CN107393671B CN107393671B CN201710479922.9A CN201710479922A CN107393671B CN 107393671 B CN107393671 B CN 107393671B CN 201710479922 A CN201710479922 A CN 201710479922A CN 107393671 B CN107393671 B CN 107393671B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0213—Manufacturing of magnetic circuits made from strip(s) or ribbon(s)
Abstract
The present invention relates to high frequency inverter technical fields, more particularly to a kind of iron based nanocrystalline magnet core and preparation method thereof, the iron based nanocrystalline magnet core is by iron based nano crystal strip coil around forming, the iron based nano crystal band includes the element of following weight percent: Si:14%-16%, B:7%-9%, Nb:1%-3%, Cu:1.6%-1.8%, Zr:4%-6%, Al:0.5%-1.5%, surplus Fe.Iron based nanocrystalline magnet core of the invention has many advantages, such as stable magnetic conductivity and direct current biasing ability, also has high saturated magnetic induction, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
Description
Technical field
The present invention relates to high frequency inverter technical fields, and in particular to a kind of iron based nanocrystalline magnet core and its preparation side
Method.
Background technique
Soft magnetic materials is the magnetic material with low-coercivity and high magnetic permeability, and soft magnetic materials is easy to magnetize, and is also easy to move back
Magnetic, so being widely used in electrical equipment and electronic equipment.Wherein, Fe-based amorphous alloy is as a kind of currently used iron
Core soft magnetic materials is mainly made of Fe element and Si, B metalloid element, it has high saturated magnetic induction, high magnetic permeability
The features such as with low core loss, can be widely applied to distribution transformer, high power switching power supply, pulse transformer, magnetic amplifier,
Intermediate-frequency transformer and inverter iron core.
Application No. is a kind of low magnetic conduction magnetic core and its manufacturing method are disclosed in the patent application document of CN103258612A
With purposes, which is iron-based non-crystalline, and between 500~5000, the value of coercivity magnetic field strength is less than magnetic conductivity
10Am-1, annealing temperature when prepared by magnetic core material is 350 DEG C~500 DEG C, and annealing time is within 2h.Due to iron-based non-crystalline
The magnetic core magnetostriction coefficient of material is higher, simultaneously because annealing temperature when preparation is lower, annealing time is shorter, to make
Stress heat treatment is not enough, and then stress is caused not completely eliminate, and affects the linearity of the magnetic conductivity of permanent magnetic conduction；Separately
Outside, since the magnetic conductivity of the magnetic core is lower, and soft magnetic characteristic such as coercivity is higher, and core loss is larger, is not suitable for high frequency
In the use environment of high inductance.
With new electronic industry development, more higher requirements, such as photovoltaic, wind-powered electricity generation, change are proposed to soft magnetic materials
The progress of the inverters such as frequency dragging, proposes with high inductance, high anti-saturation the key components inductance of electromagnetic compatibility
The requirement such as performance, excellent frequency characteristic of MHz grade, therefore on the basis of iron-based non-crystalline material, iron-base nanometer crystal alloy
It comes into being.The elements such as a small amount of Nb, Cu, Si, B are added based on ferro element in such alloy.The conjunction that above-mentioned element is constituted
Gold can be initially formed a kind of amorphous material through fast solidification technology, which can get using after crystallization and thermal treatment
Diameter is the nanocrystal main phase of 10~20nm, while also retaining a small amount of amorphous residual phase, overall to be referred to as nanocrystalline material.
Nanocrystalline material has the comprehensive magnetics energy such as high saturated magnetic induction, high initial magnetoconductivity and low-coercivity, nanocrystalline material
Manufactured magnetic core has very low core loss under high frequency, high magnetic strength, and has minimum magnetostriction coefficient and pole
Strong induced anisotropy constant Ku, by vertical or horizontal magnetic field processing after, can be obtained high residual magnetic flux density value or
The magnetic core of low residual magnetic flux density value can be widely applicable in different frequency ranges.Nanocrystalline magnet core is widely used in greatly
Power switch power source, inverter, magnetic amplifier, high frequency transformer, high-frequency converter, high frequency choke coil iron core, Current Mutual Inductance
In device iron core, earth leakage circuit-breaker and common mode inductance iron core.
Existing magnetic core product main cored, sendust core, iron nickel magnetic core, MPP magnetic core etc..Conventional iron core valence
It is honest and clean, but comprehensive performance is poor.
Summary of the invention
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of iron based nano crystals
Magnetic core, the iron based nanocrystalline magnet core have stable magnetic conductivity and direct current biasing ability, also have high saturated magnetic induction, low
The advantages that loss value, low-coercivity, high temperature resistant, high comprehensive performance.
Another object of the present invention is to provide a kind of preparation method of iron based nanocrystalline magnet core, the preparation method technique letters
Single, convenient operation and control, quality is stablized, and high production efficiency, production cost is low, can large-scale industrial production.
The purpose of the invention is achieved by the following technical solution: a kind of iron based nanocrystalline magnet core, the iron based nano crystal magnetic
For core by iron based nano crystal strip coil around forming, the iron based nano crystal band includes the element of following weight percent: Si:14%-
16%, B:7%-9%, Nb:1%-3%, Cu:1.6%-1.8%, Zr:4%-6%, Al:0.5%-1.5%, surplus Fe.
Amorphous formation elements Si, B, Fe-based nanocrystalline magnetically soft alloy are typically all to pass through conjunction on amorphous alloy basis
Suitable subsequent annealing forms it into nanocrystalline material, thus decrystallized element is basic component, especially B element, former
Sub- radius is smaller, and outer-shell electron is more, is very beneficial for forming amorphous alloy, Si is also important decrystallized element, in this hair
In bright, si content be higher than 18at% reduces the saturation magnetization of alloy, and si content be lower than 7at% be then not easy to be formed it is non-
Crystalline state, meanwhile, the constitution element of Si element or α-Fe (Si) nanometer crystal phase；
Nanocrystalline formation element Cu, Nb, Cu is separated with Fe first when crystallization, the enrichment region of the metallic element is formed, to receive
Meter Jing Hua plays forming core, and Nb elements diffusion is slow, and main function is to hinder growing up for α-Fe crystal grain, to guarantee crystallite dimension
In nanometer scale, the control of Cu, Nb content is for keeping the heterogeneous microstructure of magnetic core extremely important.
It Cu element is added can form high density α phase in the subsequent Amorphous Crystallization initial stage and crystallize nucleus, using as receiving
The organic centre of rice size crystal.
Iron based nanocrystalline magnet core of the invention replaces the noble metal Nb in magnetic core, addition Nb to be conducive to improve using the part Al
The Saturation magnetic sense intensity of magnetic core, addition Al is conducive to coercitive reduction, while can be substantially reduced the production cost of magnetic core.
Iron based nano crystal band of the invention is by using above-mentioned element, and the weight percent of each raw material of strict control,
Iron based nanocrystalline magnet core obtained has stable magnetic conductivity and direct current biasing ability, also has high saturated magnetic induction, low
The advantages that loss value, low-coercivity, high temperature resistant, high comprehensive performance.
Preferably, the iron based nano crystal band further includes Ga:0.4%-0.8%, V:0.1%-0.5% and Ti:0.2%-
0.6%。
Iron based nano crystal band of the invention is by increasing Ga, V and Ti element, and the weight percent of each raw material of strict control
Than the first time crystallization temperature of alloy can be improved, to reduce the gap between crystallization temperature twice.
Preferably, the iron based nano crystal band further includes Mn:1%-3%, Cr:0.5%-1.5% and Mo:0.8%-1.2%.
Iron based nano crystal band of the invention is by increasing Mn, Cr and Mo element, and the weight hundred of each raw material of strict control
Divide ratio, material can be made to form stronger annealing induced anisotropy constant, forms controllable adjustment during horizontal magnetic anneal
Lateral magnetic anisotropy, to reach the characteristic of linear magnetic conductivity and anti-saturation.
Preferably, the iron based nano crystal band further includes C:1.2%-1.4%, Ge:0.01%-0.05% and P:0.001%-
0.005%。
Iron based nano crystal band of the invention is by increasing C, Ge and P element, and the weight percent of each raw material of strict control
Than the first time crystallization temperature of alloy can be improved, to reduce the gap between crystallization temperature twice.
Preferably, the iron based nano crystal band further includes Vb:1.4%-1.8%, Ta:0.3%-0.7% and W:0.04%-
0.08%。
Iron based nano crystal band of the invention is by increasing Vb, Ta and W element, and the weight percent of each raw material of strict control
Than nanocrystalline crystal grain can be prevented to grow up, maintain and ultimately form nanoscale crystalline size structure.
A kind of preparation method of iron based nanocrystalline magnet core, includes the following steps:
(1) the iron based nano crystal band raw material of said components is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
Preferably, in the step (3), iron based nano crystal band with a thickness of 15-25 μm, width 20-30mm.This hair
The bright thickness and width by strictly controlling iron-based nanocrystalline strip processed, so that iron based nanocrystalline magnet core is keeping good inductance
While amount, higher quality factor, the loss value of product is reduced, direct current biasing ability is improved.
Preferably, in the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 110-130min in-furnace temperature from room temperature to 640-660K；
B) after 643-663K keeps the temperature 15-25min, 750-770K is warming up to 32-40min；
C) after 753-773K keeps the temperature 35-45min, 790-810K is warming up to 11-15min；
D) after 793-813K keeps the temperature 55-65min, 825-845K is warming up to 10-14min；
E) after 828-848K keeps the temperature 35-45min, bonnet high wind is exited furnace body temperature and is chilled to 340-360K, open
Firedoor handle nanocrystalline magnet core takes out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
The nanocrystalline magnet core to be heat-treated is passed through identical heat twice by the conventional lattice annealing furnace of annealing process of the invention
Treatment process simplifies heat treatment process, simple process subtracts to reach the electrical requirements that horizontal magnetic furnace reduces nanocrystalline magnet core Br
Production equipment investment is lacked, 25% or more power cost can also have been saved, production cost is low.Annealing process system through the invention
Nanocrystalline magnet core have stable magnetic conductivity and direct current biasing ability, also have high saturated magnetic induction, low loss-value,
The advantages that low-coercivity, high temperature resistant, high comprehensive performance.
Preferably, in the step (4) and the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, very
Filled with mixed gas in empty annealing furnace, the hydrogen and percent by volume that mixed gas is 10%-20% by percent by volume are 80%-
90% nitrogen composition.
The present invention is filled with nitrogen and hydrogen mixture by the vacuum degree in strict control vacuum annealing furnace in vacuum annealing furnace
The magnetic conductivity of nanocrystalline magnet core can be improved in body.After injecting nitrogen, nitrogen primarily serves the effect of uniform temperature, and nitrogen is exactly
The transmitting medium of heat makes furnace inner magnetic core uniformly be heated, thus make magnetic core temperature uniformly, balance, the magnetic of nanocrystalline magnet core
Conductance is related in atmosphere of annealing furnace, and when the atmosphere difference of annealing furnace, magnetic conductivity has certain difference；Through overtesting obtain with
Draw a conclusion, the magnetic conductivity changing rule of magnetic core is: better than before not vacuumizing after vacuumizing in annealing furnace；It vacuumizes again
It is filled with nitrogen hydrogen mixeding gas, is got well than only vacuumizing.
Preferably, the step (5) further includes that the nanocrystalline magnet core after step (6) will be heat-treated again carries out later
Impregnation curing process.
In the step (6), impregnation curing process includes the following steps:
A, nanocrystalline magnet core is preheated at a temperature of 60-70 DEG C；
B, using epoxy resin shellac varnish as curing agent, epoxy resin shellac varnish is heated under 60-70 DEG C of environment of water-bath；And
Dilution is dissolved so that the ratio of shellac varnish and diluent is 0.8-1.2:1 with diluent, the shellac varnish after dilution is kept the temperature at 60-70 DEG C
40-80min；
C, the nanocrystalline magnet core after preheating is dipped in the hot glue paint after dissolving, by the way of vacuum impregnation, is impregnated with 30-
50min, vacuum degree 0.6-0.8Mpa；
D, by the nanocrystalline magnet core after impregnation using three sections of thermal-insulating method solidifications, 60-80 DEG C of first segment temperature keeps the temperature 40-
80min；100-120 DEG C of second segment temperature keeps the temperature 80-120min；140-160 DEG C of temperature of third section, keep the temperature 80-120min；From
It is so cooling.
For the curing mode for solving the problems, such as nanocrystalline magnet core, the curing schedule of this method uses high-adhesive-strength, low answers
The molding of power glue curing, i.e. epoxy resin shellac varnish.Shellac varnish and nanocrystalline magnet core are first preheated before impregnation, so that the temperature of the two is protected
It holds at 60-70 DEG C, when epoxy resin shellac varnish is at 70 DEG C or so, activity increases, and viscosity can decline, ensure that drenching in this way
When glue, extra shellac varnish can flow out the inside of nanocrystalline magnet core by the gravity of itself, ensure that the table of nanocrystalline magnet core
Face is clean, does not influence the subsequent cutting accuracy of magnetic core.Secondly, the viscosity further to improve shellac varnish and the flowing after heating
Property, use acetone for diluent, shellac varnish and diluent are dissolved with the ratio of 0.8-1.2:1.And using three sections of guarantors after being impregnated with
Warm therapy solidification makes the shellac varnish dissolved form sealing film in nanocrystalline magnetic wicking surface in the event of high temperatures, guarantees that shellac varnish remains in
Nanocrystalline magnetic core inner, solve existing usual manner paint leakage and intensity it is low the problems such as, while shellac varnish high intensity and
Low stress plays the role of power-assisted to the not damaged and mirror surface requirement finally cut.
The beneficial effects of the present invention are: iron based nanocrystalline magnet core of the invention has stable magnetic conductivity and direct current biasing
Ability also has many advantages, such as high saturated magnetic induction, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
Preparation method simple process of the invention, convenient operation and control, quality are stablized, and high production efficiency, production cost is low,
It can large-scale industrial production.
Specific embodiment
For the ease of the understanding of those skilled in the art, below with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1
A kind of iron based nanocrystalline magnet core, the iron based nanocrystalline magnet core by iron based nano crystal strip coil around forming, the iron
Base nanometer crystal band includes the element of following weight percent: Si:14%, B:7%, Nb:1%, Cu:1.6%, Zr:4%, Al:0.5%,
Surplus is Fe.
The iron based nano crystal band further include Ga:0.4%, V:0.1%, Ti:0.2, Mn:1%, Cr:0.5%, Mo:0.8%,
C:1.2%, Ge:0.01%, P:0.001%, Vb:1.4%, Ta:0.3% and W:0.04%.
A kind of preparation method of iron based nanocrystalline magnet core, includes the following steps:
(1) the iron based nano crystal band raw material of said components is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (3), iron based nano crystal band with a thickness of 15 μm, width 20mm.
In the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 110min in-furnace temperature from room temperature to 640K；
B) after 643K keeps the temperature 15min, 750K is warming up to 32min；
C) after 753K keeps the temperature 35min, 790K is warming up to 11min；
D) after 793K keeps the temperature 55min, 825K is warming up to 10min；
E) after 828K keeps the temperature 35min, bonnet high wind is exited furnace body temperature and is chilled to 340K, opens firedoor handle nanometer
Brilliant magnetic core takes out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
In the step (4) and the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
It is interior filled with mixed gas, the nitrogen that the hydrogen and percent by volume that mixed gas is 10% by percent by volume are 90% forms.
The step (5) further includes that the nanocrystalline magnet core progress impregnation after step (6) will be heat-treated again is consolidated later
Change processing.
In the step (6), impregnation curing process includes the following steps:
A, nanocrystalline magnet core is preheated at a temperature of 60 DEG C；
B, using epoxy resin shellac varnish as curing agent, epoxy resin shellac varnish is heated under 60 DEG C of environment of water-bath；It is used in combination
Diluent dissolves dilution so that the ratio of shellac varnish and diluent is 0.8:1, and the shellac varnish after dilution keeps the temperature 40min at 60 DEG C；
C, the nanocrystalline magnet core after preheating is dipped in the hot glue paint after dissolving, by the way of vacuum impregnation, impregnation
30min, vacuum degree 0.6Mpa；
D, by the nanocrystalline magnet core after impregnation using three sections of thermal-insulating method solidifications, first segment temperature 60 C keeps the temperature 40min；The
Two sections 100 DEG C of temperature, keep the temperature 80min；140 DEG C of third section temperature keeps the temperature 80min；Natural cooling.
Embodiment 2
A kind of iron based nanocrystalline magnet core, the iron based nanocrystalline magnet core by iron based nano crystal strip coil around forming, the iron
Base nanometer crystal band includes the element of following weight percent: Si:14.5%, B:7.5%, Nb:1.5%, Cu:1.65%, Zr:
4.5%, Al:0.8%, surplus Fe.
The iron based nano crystal band further includes Ga:0.5%, V:0.2%, Ti:0.3%, Mn:1.5%, Cr:0.8%, Mo:
0.9%, C:1.25%, Ge:0.02%, P:0.002%, Vb:1.5%, Ta:0.4% and W:0.05%.
A kind of preparation method of iron based nanocrystalline magnet core, includes the following steps:
(1) the iron based nano crystal band raw material of said components is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (3), iron based nano crystal band with a thickness of 18 μm, width 22mm.
In the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 115min in-furnace temperature from room temperature to 645K；
B) after 648K keeps the temperature 18min, 755K is warming up to 34min；
C) after 758K keeps the temperature 38min, 795K is warming up to 12min；
D) after 798K keeps the temperature 58min, 830K is warming up to 11min；
E) after 833K keeps the temperature 38min, bonnet high wind is exited furnace body temperature and is chilled to 345K, opens firedoor handle nanometer
Brilliant magnetic core takes out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
In the step (4) and the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
It is interior filled with mixed gas, the nitrogen that the hydrogen and percent by volume that mixed gas is 12% by percent by volume are 88% forms.
The step (5) further includes that the nanocrystalline magnet core progress impregnation after step (6) will be heat-treated again is consolidated later
Change processing.
In the step (6), impregnation curing process includes the following steps:
A, nanocrystalline magnet core is preheated at a temperature of 62 DEG C；
B, using epoxy resin shellac varnish as curing agent, epoxy resin shellac varnish is heated under 62 DEG C of environment of water-bath；It is used in combination
Diluent dissolves dilution so that the ratio of shellac varnish and diluent is 0.9:1, and the shellac varnish after dilution keeps the temperature 50min at 62 DEG C；
C, the nanocrystalline magnet core after preheating is dipped in the hot glue paint after dissolving, by the way of vacuum impregnation, impregnation
35min, vacuum degree 0.65Mpa；
D, the nanocrystalline magnet core after impregnation 65 DEG C of first segment temperature, is kept the temperature into 50min using three sections of thermal-insulating method solidifications；The
Two sections 105 DEG C of temperature, keep the temperature 90min；145 DEG C of third section temperature keeps the temperature 90min；Natural cooling.
Embodiment 3
A kind of iron based nanocrystalline magnet core, the iron based nanocrystalline magnet core by iron based nano crystal strip coil around forming, the iron
Base nanometer crystal band includes the element of following weight percent: Si:15%, B:8%, Nb:2%, Cu:1.7%, Zr:5%, Al:1.0%,
Surplus is Fe.
The iron based nano crystal band further include Ga:0.6%, V:0.3%, Ti:0.4%, Mn:2%, Cr:1.0%, Mo:1.0%,
C:1.3%, Ge:0.03%, P:0.003%, Vb:1.6%, Ta:0.5% and W:0.06%.
A kind of preparation method of iron based nanocrystalline magnet core, includes the following steps:
(1) the iron based nano crystal band raw material of said components is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (3), iron based nano crystal band with a thickness of 20 μm, width 25mm.
In the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 120min in-furnace temperature from room temperature to 650K；
B) after 653K keeps the temperature 20min, 760K is warming up to 36min；
C) after 763K keeps the temperature 40min, 800K is warming up to 13min；
D) after 803K keeps the temperature 60min, 835K is warming up to 12min；
E) after 838K keeps the temperature 40min, bonnet high wind is exited furnace body temperature and is chilled to 350K, opens firedoor handle nanometer
Brilliant magnetic core takes out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
In the step (4) and the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
It is interior filled with mixed gas, the nitrogen that the hydrogen and percent by volume that mixed gas is 15% by percent by volume are 85% forms.
The step (5) further includes that the nanocrystalline magnet core progress impregnation after step (6) will be heat-treated again is consolidated later
Change processing.
In the step (6), impregnation curing process includes the following steps:
A, nanocrystalline magnet core is preheated at a temperature of 65 DEG C；
B, using epoxy resin shellac varnish as curing agent, epoxy resin shellac varnish is heated under 65 DEG C of environment of water-bath；It is used in combination
Diluent dissolves dilution so that the ratio of shellac varnish and diluent is 1:1, and the shellac varnish after dilution keeps the temperature 60min at 65 DEG C；
C, the nanocrystalline magnet core after preheating is dipped in the hot glue paint after dissolving, by the way of vacuum impregnation, impregnation
40min, vacuum degree 0.7Mpa；
D, by the nanocrystalline magnet core after impregnation using three sections of thermal-insulating method solidifications, first segment temperature 70 C keeps the temperature 60min；The
Two sections 110 DEG C of temperature, keep the temperature 810min；150 DEG C of third section temperature keeps the temperature 100min；Natural cooling.
Embodiment 4
A kind of iron based nanocrystalline magnet core, the iron based nanocrystalline magnet core by iron based nano crystal strip coil around forming, the iron
Base nanometer crystal band includes the element of following weight percent: Si:15.5%, B:8.5%, Nb:2.5%, Cu:1.75%, Zr:
5.5%, Al:1.2%, surplus Fe.
The iron based nano crystal band further includes Ga:0.7%, V:0.4%, Ti:0.5%, Mn:2.5%, Cr:1.2%, Mo:
1.1%, C:1.35%, Ge:0.04%, P:0.004%, Vb:1.7%, Ta:0.6% and W:0.07%.
A kind of preparation method of iron based nanocrystalline magnet core, includes the following steps:
(1) the iron based nano crystal band raw material of said components is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (3), iron based nano crystal band with a thickness of 22 μm, width 28mm.
In the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 125min in-furnace temperature from room temperature to 655K；
B) after 658K keeps the temperature 22min, 765K is warming up to 38min；
C) after 768K keeps the temperature 42min, 805K is warming up to 14min；
D) after 808K keeps the temperature 62min, 840K is warming up to 13min；
E) after 843K keeps the temperature 42min, bonnet high wind is exited furnace body temperature and is chilled to 355K, opens firedoor handle nanometer
Brilliant magnetic core takes out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
In the step (4) and the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
It is interior filled with mixed gas, the nitrogen that the hydrogen and percent by volume that mixed gas is 18% by percent by volume are 82% forms.
The step (5) further includes that the nanocrystalline magnet core progress impregnation after step (6) will be heat-treated again is consolidated later
Change processing.
In the step (6), impregnation curing process includes the following steps:
A, nanocrystalline magnet core is preheated at a temperature of 68 DEG C；
B, using epoxy resin shellac varnish as curing agent, epoxy resin shellac varnish is heated under 68 DEG C of environment of water-bath；It is used in combination
Diluent dissolves dilution so that the ratio of shellac varnish and diluent is 1.1:1, and the shellac varnish after dilution keeps the temperature 70min at 68 DEG C；
C, the nanocrystalline magnet core after preheating is dipped in the hot glue paint after dissolving, by the way of vacuum impregnation, impregnation
45min, vacuum degree 0.75Mpa；
D, the nanocrystalline magnet core after impregnation 75 DEG C of first segment temperature, is kept the temperature into 70min using three sections of thermal-insulating method solidifications；The
Two sections 115 DEG C of temperature, keep the temperature 110min；155 DEG C of third section temperature keeps the temperature 110min；Natural cooling.
Embodiment 5
A kind of iron based nanocrystalline magnet core, the iron based nanocrystalline magnet core by iron based nano crystal strip coil around forming, the iron
Base nanometer crystal band includes the element of following weight percent: Si:16%, B:9%, Nb:3%, Cu:1.8%, Zr:6%, Al:1.5%,
Surplus is Fe.
The iron based nano crystal band further include Ga:0.8%, V:0.5%, Ti:0.6%, Mn:3%, Cr:1.5%, Mo:1.2%,
C:1.4%, Ge:0.05%, P:0.005%, Vb:1.8%, Ta:0.7% and W:0.08%.
A kind of preparation method of iron based nanocrystalline magnet core, includes the following steps:
(1) the iron based nano crystal band raw material of said components is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (3), iron based nano crystal band with a thickness of 25 μm, width 30mm.
In the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 130min in-furnace temperature from room temperature to 660K；
B) after 663K keeps the temperature 25min, 770K is warming up to 40min；
C) after 773K keeps the temperature 45min, 810K is warming up to 15min；
D) after 813K keeps the temperature 65min, 845K is warming up to 14min；
E) after 848K keeps the temperature 45min, bonnet high wind is exited furnace body temperature and is chilled to 360K, opens firedoor handle nanometer
Brilliant magnetic core takes out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
In the step (4) and the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
It is interior filled with mixed gas, the nitrogen that the hydrogen and percent by volume that mixed gas is 20% by percent by volume are 80% forms.
The step (5) further includes that the nanocrystalline magnet core progress impregnation after step (6) will be heat-treated again is consolidated later
Change processing.
In the step (6), impregnation curing process includes the following steps:
A, nanocrystalline magnet core is preheated at a temperature of 70 DEG C；
B, using epoxy resin shellac varnish as curing agent, epoxy resin shellac varnish is heated under 70 DEG C of environment of water-bath；It is used in combination
Diluent dissolves dilution so that the ratio of shellac varnish and diluent is 1.2:1, and the shellac varnish after dilution keeps the temperature 80min at 70 DEG C；
C, the nanocrystalline magnet core after preheating is dipped in the hot glue paint after dissolving, by the way of vacuum impregnation, impregnation
50min, vacuum degree 0.8Mpa；
D, the nanocrystalline magnet core after impregnation 80 DEG C of first segment temperature, is kept the temperature into 80min using three sections of thermal-insulating method solidifications；The
Two sections 120 DEG C of temperature, keep the temperature 120min；160 DEG C of third section temperature keeps the temperature 120min；Natural cooling.
After tested, the Effective permeability μ e of nanocrystalline magnet core produced by the present invention can achieve 8.8 × 104More than, saturation
Magnetic induction value Bs can achieve 1.48T or more, and the value of coercivity magnetic field strength Hc is less than 2Am-1, remanence ratio resists straight less than 0.08
Stream biasing ability is strong, and under 100Oe field strength, magnetic conductivity still has 76% or more, wherein loss value under the conditions of 0.2T, 20k Hz
For 1.1W/kg hereinafter, magnetic core loss value under the conditions of 0.5T, 20k Hz is 5.4W/kg hereinafter, magnetic core is in 0.5T, 50k simultaneously
Loss value is 16.4W/kg or less under the conditions of Hz.
Iron based nanocrystalline magnet core of the invention has stable magnetic conductivity and direct current biasing ability, also has high saturation magnetic induction
The advantages that answering intensity, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other way,
Do not depart under the premise of present inventive concept it is any obviously replace it is within the scope of the present invention.
Claims (8)
1. a kind of preparation method of iron based nanocrystalline magnet core, it is characterised in that: the iron based nanocrystalline magnet core is by iron based nano crystal
For strip coil around forming, the iron based nano crystal band includes the element of following weight percent: Si:14%-16%, B:7%-
9%, Nb:1%-3%, Cu:1.6%-1.8%, Zr:4%-6%, Al:0.5%-1.5%, surplus Fe；
The preparation method of the iron based nanocrystalline magnet core includes the following steps:
(1) iron based nano crystal band raw material is smelted, obtains alloy melt；
(2) alloy melt is carried out by spray using single roller chilling method, obtains iron based nano crystal band；
(3) iron based nano crystal band is wound into circular nano crystalline substance magnetic core；
(4) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(5) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again；
In the step (4) and the step (5), the step of heat treatment are as follows:
A) pass through 110-130min in-furnace temperature from room temperature to 640-660K；
B) after 643-663K keeps the temperature 15-25min, 750-770K is warming up to 32-40min；
C) after 753-773K keeps the temperature 35-45min, 790-810K is warming up to 11-15min；
D) after 793-813K keeps the temperature 55-65min, 825-845K is warming up to 10-14min；
E) after 828-848K keeps the temperature 35-45min, bonnet high wind is exited furnace body temperature and is chilled to 340-360K, opens fire door
Nanocrystalline magnet core is taken out；
F) nanocrystalline magnet core taken out out of furnace is placed on cooling frame again that high wind is chilled to room temperature.
2. a kind of preparation method of iron based nanocrystalline magnet core according to claim 1, it is characterised in that: the step (3)
In, iron based nano crystal band with a thickness of 15-25 μm, width 20-30mm.
3. a kind of preparation method of iron based nanocrystalline magnet core according to claim 1, it is characterised in that: the step (4)
In the step (5), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, and vacuum annealing furnace is interior filled with mixed gas, mixing
The nitrogen that the hydrogen and percent by volume that gas is 10%-20% by percent by volume are 80%-90% forms.
4. a kind of preparation method of iron based nanocrystalline magnet core according to claim 1, it is characterised in that: the step (5)
It later further include the nanocrystalline magnet core progress impregnation curing process after step (6) will be heat-treated again.
5. a kind of iron based nanocrystalline magnet core, it is characterised in that: the iron based nanocrystalline magnet core uses claim 1-4 any one
The method is made.
6. a kind of iron based nanocrystalline magnet core according to claim 5, it is characterised in that: the iron based nano crystal band also wraps
Include Ga:0.4%-0.8%, V:0.1%-0.5% and Ti:0.2%-0.6%.
7. a kind of iron based nanocrystalline magnet core according to claim 5, it is characterised in that: the iron based nano crystal band also wraps
Include Mn:1%-3%, Cr:0.5%-1.5% and Mo:0.8%-1.2%.
8. a kind of iron based nanocrystalline magnet core according to claim 5, it is characterised in that: the iron based nano crystal band also wraps
Include C:1.2%-1.4%, Ge:0.01%-0.05% and P:0.001%-0.005%.
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| CN112117116B (en) * | 2020-10-12 | 2022-03-08 | 深圳市新核瑞科技有限公司 | Method for manufacturing iron-based or nickel-based annular magnetic core |
| CN114959213A (en) * | 2022-04-13 | 2022-08-30 | 宁波中科毕普拉斯新材料科技有限公司 | Heat treatment method of high-frequency low-loss iron-based nanocrystalline magnetic core |
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