CN107393672A - A kind of iron nickel base nanometer crystalline substance magnetic core and preparation method thereof - Google Patents
A kind of iron nickel base nanometer crystalline substance magnetic core and preparation method thereof Download PDFInfo
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- CN107393672A CN107393672A CN201710480272.XA CN201710480272A CN107393672A CN 107393672 A CN107393672 A CN 107393672A CN 201710480272 A CN201710480272 A CN 201710480272A CN 107393672 A CN107393672 A CN 107393672A
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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
- H01F1/14708—Fe-Ni based alloys
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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 field, and in particular to a kind of iron nickel base nanometer crystalline substance magnetic core and preparation method thereof, the iron nickel base nanometer crystalline substance magnetic core are made up of iron-nickel alloy, and the iron nickel base nanometer crystal zone material includes the element of following percentage by weight：Ni：15%‑25%、Si：10%‑12%、B：3%‑5%、Nb：2%‑4%、Cu：0.3%‑0.5%、Co：4% 8%, surplus Fe.The iron nickel base nanometer crystalline substance magnetic core of the present invention has stable magnetic conductivity and direct current biasing ability, also has the advantages that 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 field, and in particular to a kind of iron nickel base nanometer crystalline substance magnetic core and its preparation side
Method.
Background technology
Soft magnetic materials is the magnetic material for having 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, mainly it is made up of Fe elements 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.
A kind of low magnetic conduction magnetic core and its manufacture method are disclosed in Application No. CN103258612A patent application document
With purposes, the magnetic core material is iron-based non-crystalline, and between 500~5000, the value of coercivity magnetic field intensity 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 preparing is relatively low, annealing time is shorter, so that going
Stress heat treatment is not abundant enough, and then causes stress not to be completely eliminated, and have impact on the linearity of the magnetic conductivity of permanent magnetic conduction；Separately
Outside, because the magnetic conductivity of the magnetic core is relatively low, 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, is proposed with high inductance, high anti-saturation to the key componentses inductance of electromagnetic compatibility
The requirement such as performance, excellent frequency characteristic of MHz levels, therefore on the basis of iron-based non-crystalline material, iron-base nanometer crystal alloy
Arise at the historic moment.Such alloy adds the elements such as a small amount of Nb, Cu, Si, B based on ferro element.The conjunction that above-mentioned element is formed
Gold can be initially formed a kind of amorphous material through fast solidification technology, and the amorphous material can obtain after crystallization and thermal treatment again
A diameter of 10~20nm nanocrystal principal phase, while also retain a small amount of amorphous residual phase, it is overall to be referred to as nanocrystalline material.
Nanocrystalline material has the comprehensive magnetic 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 handle after, can obtain high residual magnetic flux density value or
The magnetic core of low residual magnetic flux density value, can widely it be 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 cores etc..Conventional iron nickel magnetic core
There is splendid frequency characteristic in 1MHz frequency range, and be lost relatively low, there is highest direct current biasing ability, produce
Moral character can be good.But also having 50% nickel in iron nickel magnetic core, price is high, and production cost is high.
The content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of iron nickel base nanometer
Brilliant magnetic core, the iron nickel base nanometer crystalline substance magnetic core has stable magnetic conductivity and direct current biasing ability, also strong with high-saturation magnetic induction
The advantages that degree, low 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 nickel base nanometer crystalline substance magnetic core, the preparation method technique
Simply, convenient operation and control, steady quality, production efficiency is high, and production cost is low, can large-scale industrial production.
The purpose of the present invention is achieved through the following technical solutions：A kind of iron nickel base nanometer crystalline substance magnetic core, the iron nickel base nanometer
Brilliant magnetic core is made up of iron-nickel alloy, and the iron nickel base nanometer crystal zone material includes the element of following percentage by weight：Ni：15%-25%、
Si：10%-12%、B：3%-5%、Nb：2%-4%、Cu：0.3%-0.5%、Co：4%-8%, surplus Fe.
Amorphous formation elements Si, B, Fe-based nanocrystalline magnetically soft alloy are typically all on amorphous alloy basis, pass through conjunction
Suitable subsequent annealing forms it into nanocrystalline material, thus decrystallized element is basic component, particularly B element, and it is 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 reduces the saturation magnetization for making alloy higher than 18at%, and si content be then not easy to be formed less than 7at% it is non-
Crystalline state, meanwhile, the constitution element of Si elements or α-Fe (Si) nanometer crystalline phase；
Nanocrystalline formation element Cu, Nb, Cu separates with Fe first during crystallization, forms the enrichment region of the metallic element, to be nanocrystalline
Forming core effect is changed, Nb elements diffusions are slow, and main function is to hinder growing up for α-Fe crystal grain, so as to ensure that crystallite dimension is being received
Rice magnitude, the control of Cu, Nb content is for keeping the heterogeneous microstructure of magnetic core extremely important.
Nucleus can be crystallized in subsequent Amorphous Crystallization starting stage formation high density α phases by adding Cu elements, to make
For the organic centre of nm-sized crystalline.
The iron nickel base nanometer crystalline substance magnetic core of the present invention has made improvement on the formula of traditional iron based nanocrystalline magnet core, increases
The metallic nickel of proper proportion, the nanocrystalline magnet core prepared have more preferably toughness, temperature tolerance and permeability.
With Co elements replace part Fe in the iron nickel base nanometer crystalline substance magnetic core of the present invention, can significantly improve magnetic core high temperature,
High frequency characteristics and quality factor, the Curie temperature of magnetic core, the intensity of magnetization before Co replacement of fe than significantly improving.
The iron nickel base nanometer crystalline substance magnetic core of the present invention is favourable using the noble metal Nb in Al, Ni part substitution magnetic core, addition Nb
In the Saturation magnetic sense intensity for improving magnetic core, addition Al is advantageous to coercitive reduction, while can substantially reduce the production of magnetic core
Cost.
The iron nickel base nanometer crystal zone material of the present invention strictly controls the weight percent of each raw material by using above-mentioned element
Than obtained iron nickel base nanometer crystalline substance magnetic core has stable magnetic conductivity and direct current biasing ability, also strong with high-saturation magnetic induction
The advantages that degree, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
Preferably, the iron nickel base nanometer crystal zone material also includes Ga：0.4%-0.8%、V：0.1%-0.5% and Ti：0.2%-
0.6%。
The iron nickel base nanometer crystal zone material of the present invention strictly controls the weight hundred of each raw material by increasing Ga, V and Ti element
Divide ratio, the first time crystallization temperature of alloy can be improved, so as to reduce the gap between crystallization temperature twice.
Preferably, the iron nickel base nanometer crystal zone material also includes Mn：1%-3%、Cr：0.5%-1.5% and Mo：0.8%-1.2%.
The iron nickel base nanometer crystal zone material of the present invention strictly controls the weight of each raw material by increasing Mn, Cr and Mo element
Percentage, material can be made to form stronger annealing induced anisotropy constant, controllable adjustment is formed during horizontal magnetic anneal
Horizontal magnetic anisotropy, to reach the characteristic of linear magnetic conductivity and anti-saturation.
Preferably, the iron nickel base nanometer crystal zone material also includes C：1.2%-1.4%、Ge：0.01%-0.05% and P：
0.001%-0.005%。
The iron nickel base nanometer crystal zone material of the present invention strictly controls the weight hundred of each raw material by increasing C, Ge and P element
Divide ratio, the first time crystallization temperature of alloy can be improved, so as to reduce the gap between crystallization temperature twice.
Preferably, the iron nickel base nanometer crystal zone material also includes Vb：1.4%-1.8%、Ta：0.3%-0.7% and W：0.04%-
0.08%。
The iron nickel base nanometer crystal zone material of the present invention strictly controls the weight hundred of each raw material by increasing Vb, Ta and W element
Divide ratio, nanocrystalline crystal grain can be prevented to grow up, maintain and ultimately form nano level crystalline size structure.
A kind of preparation method of iron nickel base nanometer crystalline substance magnetic core, comprises the following steps：
（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；
（3）Iron nickel base nanometer crystal zone material 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, the step（3）In, the thickness of iron nickel base nanometer crystal zone material is 15-25 μm, width 20-30mm.This
The thickness and width that invention passes through strictly control iron nickel base nanometer crystal zone material so that iron nickel base nanometer crystalline substance magnetic core is being kept well
While inductance value, higher quality factor, the loss value of product is reduced, improves direct current biasing ability.
Preferably, the step（4）With the step（5）In, it is the step of heat treatment：
A) 110-130min is passed through in-furnace temperature from room temperature to 640-660K；
B) after 643-663K is incubated 15-25min, 750-770K is warming up to 32-40min；
C) after 753-773K is incubated 35-45min, 790-810K is warming up to 11-15min；
D) after 793-813K is incubated 55-65min, 825-845K is warming up to 10-14min；
E) after 828-848K is incubated 35-45min, exit bonnet high wind and furnace body temperature is chilled to 340-360K, open fire door
Nanocrystalline magnet core is taken out；
F) nanocrystalline magnet core taken out out of stove is placed on cooling frame again that high wind is chilled to normal temperature.
The nanocrystalline magnet core to be heat-treated is passed through identical heat twice by the annealing process of the present invention with conventional lattice annealing furnace
Handling process simplifies Technology for Heating Processing, technique is simple, subtracts to reach the electrical requirements that horizontal magnetic stove reduces nanocrystalline magnet core Br
Production equipment input is lacked, power cost more than 25% can also have been saved, production cost is low.Pass through the annealing process system of the present invention
Nanocrystalline magnet core there is stable magnetic conductivity and direct current biasing ability, also with high saturated magnetic induction, low loss-value,
The advantages that low-coercivity, high temperature resistant, high comprehensive performance.
Preferably, the step（4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, very
Filled with mixed gas in empty annealing furnace, 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 strictly controlling the vacuum in vacuum annealing furnace in vacuum annealing furnace
Body, the magnetic conductivity of nanocrystalline magnet core can be improved.After injecting nitrogen, nitrogen primarily serves the effect of uniform temperature, and nitrogen is exactly
The transmitting medium of heat, stove inner magnetic core is set uniformly to be heated, so that the temperature of magnetic core is uniform, balance, the magnetic of nanocrystalline magnet core
Conductance is relevant with atmosphere of annealing furnace, and during the atmosphere difference of annealing furnace, magnetic conductivity has certain difference；Through overtesting draw with
Draw a conclusion, the magnetic conductivity changing rule of magnetic core is：It is better than before not vacuumizing after vacuumizing in annealing furnace；Vacuumize again
Nitrogen hydrogen mixeding gas are filled with, it is better than only vacuumizing.
Preferably, the step（5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again is carried out
Impregnation curing process.
The step（6）In, impregnation curing process comprises the following steps：
A, nanocrystalline magnet core is preheated at a temperature of 60-70 DEG C；
B, epoxy resin shellac varnish is heated under 60-70 DEG C of environment of water-bath as curing agent using epoxy resin shellac varnish；And with dilute
Agent is released using the ratio of shellac varnish and diluent as 0.8-1.2:1 dilutes to dissolve, and the shellac varnish after dilution is incubated 40- at 60-70 DEG C
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 0.6-0.8Mpa；
D, the nanocrystalline magnet core after impregnation is solidified using three sections of thermal-insulating methods, 60-80 DEG C of first paragraph temperature, is incubated 40-80min；
100-120 DEG C of second segment temperature, it is incubated 80-120min；3rd section of 140-160 DEG C of temperature, it is incubated 80-120min；Natural cooling.
To solve the problems, such as the curing mode of nanocrystalline magnet core, the curing schedule of this method employ high-adhesive-strength, it is low should
Power glue curing is molded, i.e. epoxy resin shellac varnish.Shellac varnish and nanocrystalline magnet core are first preheated before impregnation so that both temperature are protected
Hold at 60-70 DEG C, when epoxy resin shellac varnish is at 70 DEG C or so, activity increase, viscosity can decline, so ensure that and drench
During glue, unnecessary shellac varnish can flow out the inside of nanocrystalline magnet core by the Action of Gravity Field of itself, ensure that the table of nanocrystalline magnet core
Face is clean, does not influence the follow-up cutting accuracy of magnetic core.Secondly, it is the flowing after the further viscosity of improvement shellac varnish and heating
Property, acetone is used as diluent, and shellac varnish is with diluent with 0.8-1.2:1 ratio dissolves.And using three sections of guarantors after being impregnated with
Warm therapy solidifies, and the shellac varnish for making to dissolve forms diaphragm seal in nanocrystalline magnetic wicking surface in the event of high temperatures, ensures that shellac varnish remains in
Nanocrystalline magnetic core inner, solves the problems such as paint seepage and low intensity of existing usual manner, at the same the high intensity of shellac varnish and
Low stress plays power-assisted effect to the not damaged and minute surface requirement finally cut.
The beneficial effects of the present invention are：The iron nickel base nanometer crystalline substance magnetic core of the present invention has stable magnetic conductivity and direct current inclined
Ability is put, also there is high saturated magnetic induction, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
The preparation method technique of the present invention is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low,
Can large-scale industrial production.
Embodiment
For the ease of the understanding of those skilled in the art, 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 nickel base nanometer crystalline substance magnetic core, the iron nickel base nanometer crystalline substance magnetic core are made up of iron-nickel alloy, and the iron nickel base nanometer is brilliant
Band includes the element of following percentage by weight：Ni：15%、Si：10%、B：3%、Nb：2%、Cu：0.3%、Co：4%, surplus Fe.
The iron nickel base nanometer crystal zone material also includes 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 nickel base nanometer crystalline substance magnetic core, comprises the following steps：
（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；
（3）Iron nickel base nanometer crystal zone material 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.
The step（3）In, the thickness of iron nickel base nanometer crystal zone material is 15 μm, width 20mm.
The step（4）With the step（5）In, it is the step of heat treatment：
A) 110min is passed through in-furnace temperature from room temperature to 640K；
B) after 643K is incubated 15min, 750K is warming up to 32min；
C) after 753K is incubated 35min, 790K is warming up to 11min；
D) after 793K is incubated 55min, 825K is warming up to 10min；
E) after 828K is incubated 35min, exit bonnet high wind and furnace body temperature is chilled to 340K, open firedoor handle nanocrystalline magnetic
Core takes out；
F) nanocrystalline magnet core taken out out of stove is placed on cooling frame again that high wind is chilled to normal temperature.
The step（4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
The nitrogen that the interior hydrogen and percent by volume that filled with mixed gas, mixed gas is 10% by percent by volume is 90% forms.
The step（5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again carries out impregnation and consolidated
Change is handled.
The step（6）In, impregnation curing process comprises the following steps：
A, nanocrystalline magnet core is preheated at a temperature of 60 DEG C；
B, epoxy resin shellac varnish is heated under 60 DEG C of environment of water-bath as curing agent using epoxy resin shellac varnish；And with dilution
Agent is using the ratio of shellac varnish and diluent as 0.8:1 dilutes to dissolve, and the shellac varnish after dilution is incubated 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, is impregnated with 30min,
Vacuum is 0.6Mpa；
D, the nanocrystalline magnet core after impregnation is solidified using three sections of thermal-insulating methods, first paragraph temperature 60 C, is incubated 40min；Second segment
100 DEG C of temperature, it is incubated 80min；3rd section of 140 DEG C of temperature, it is incubated 80min；Natural cooling.
Embodiment 2
A kind of iron nickel base nanometer crystalline substance magnetic core, the iron nickel base nanometer crystalline substance magnetic core are made up of iron-nickel alloy, and the iron nickel base nanometer is brilliant
Band includes the element of following percentage by weight：Ni：18%、Si：11.5%、B：3.5%、Nb：2.5%、Cu：0.35%、Co：5%, it is remaining
Measure as Fe.
The iron nickel base nanometer crystal zone material also 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 nickel base nanometer crystalline substance magnetic core, comprises the following steps：
（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；
（3）Iron nickel base nanometer crystal zone material 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.
The step（3）In, the thickness of iron nickel base nanometer crystal zone material is 15-25 μm, width 20-30mm.
The step（4）With the step（5）In, it is the step of heat treatment：
A) 115min is passed through in-furnace temperature from room temperature to 645K；
B) after 648K is incubated 18min, 755K is warming up to 34min；
C) after 758K is incubated 38min, 795K is warming up to 12min；
D) after 798K is incubated 58min, 830K is warming up to 11min；
E) after 833K is incubated 38min, exit bonnet high wind and furnace body temperature is chilled to 345K, open firedoor handle nanocrystalline magnetic
Core takes out；
F) nanocrystalline magnet core taken out out of stove is placed on cooling frame again that high wind is chilled to normal temperature.
The step（4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
The nitrogen that the interior hydrogen and percent by volume that filled with mixed gas, mixed gas is 12% by percent by volume is 88% forms.
The step（5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again carries out impregnation and consolidated
Change is handled.
The step（6）In, impregnation curing process comprises the following steps：
A, nanocrystalline magnet core is preheated at a temperature of 62 DEG C；
B, epoxy resin shellac varnish is heated under 62 DEG C of environment of water-bath as curing agent using epoxy resin shellac varnish；And with dilution
Agent is using the ratio of shellac varnish and diluent as 0.9:1 dilutes to dissolve, and the shellac varnish after dilution is incubated 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, is impregnated with 35min,
Vacuum is 0.65Mpa；
D, the nanocrystalline magnet core after impregnation is solidified using three sections of thermal-insulating methods, 65 DEG C of first paragraph temperature, is incubated 50min；Second segment
105 DEG C of temperature, it is incubated 90min；3rd section of 145 DEG C of temperature, it is incubated 90min；Natural cooling.
Embodiment 3
A kind of iron nickel base nanometer crystalline substance magnetic core, the iron nickel base nanometer crystalline substance magnetic core are made up of iron-nickel alloy, and the iron nickel base nanometer is brilliant
Band includes the element of following percentage by weight：Ni：20%、Si：11%、B：4%、Nb：3%、Cu：0.4%、Co：6%, surplus Fe.
The iron nickel base nanometer crystal zone material also includes 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 nickel base nanometer crystalline substance magnetic core, comprises the following steps：
（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；
（3）Iron nickel base nanometer crystal zone material 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.
The step（3）In, the thickness of iron nickel base nanometer crystal zone material is 20 μm, width 25mm.
The step（4）With the step（5）In, it is the step of heat treatment：
A) 120min is passed through in-furnace temperature from room temperature to 650K；
B) after 653K is incubated 20min, 760K is warming up to 36min；
C) after 763K is incubated 40min, 800K is warming up to 13min；
D) after 803K is incubated 60min, 835K is warming up to 12min；
E) after 838K is incubated 40min, exit bonnet high wind and furnace body temperature is chilled to 350K, open firedoor handle nanocrystalline magnetic
Core takes out；
F) nanocrystalline magnet core taken out out of stove is placed on cooling frame again that high wind is chilled to normal temperature.
The step（4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
The nitrogen that the interior hydrogen and percent by volume that filled with mixed gas, mixed gas is 15% by percent by volume is 85% forms.
The step（5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again carries out impregnation and consolidated
Change is handled.
The step（6）In, impregnation curing process comprises the following steps：
A, nanocrystalline magnet core is preheated at a temperature of 65 DEG C；
B, epoxy resin shellac varnish is heated under 65 DEG C of environment of water-bath as curing agent using epoxy resin shellac varnish；And with dilution
Agent is using the ratio of shellac varnish and diluent as 1:1 dilutes to dissolve, and the shellac varnish after dilution is incubated 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, is impregnated with 40min,
Vacuum is 0.7Mpa；
D, the nanocrystalline magnet core after impregnation is solidified using three sections of thermal-insulating methods, first paragraph temperature 70 C, is incubated 60min；Second segment
110 DEG C of temperature, it is incubated 810min；3rd section of 150 DEG C of temperature, it is incubated 100min；Natural cooling.
Embodiment 4
A kind of iron nickel base nanometer crystalline substance magnetic core, the iron nickel base nanometer crystalline substance magnetic core are made up of iron-nickel alloy, and the iron nickel base nanometer is brilliant
Band includes the element of following percentage by weight：Ni：22%、Si：11.5%、B：4.5%、Nb：3.5%、Cu：0.45%、Co：7%, it is remaining
Measure as Fe.
The iron nickel base nanometer crystal zone material also 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 nickel base nanometer crystalline substance magnetic core, comprises the following steps：
（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；
（3）Iron nickel base nanometer crystal zone material 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.
The step（3）In, the thickness of iron nickel base nanometer crystal zone material is 22 μm, width 28mm.
The step（4）With the step（5）In, it is the step of heat treatment：
A) 125min is passed through in-furnace temperature from room temperature to 655K；
B) after 658K is incubated 22min, 765K is warming up to 38min；
C) after 768K is incubated 42min, 805K is warming up to 14min；
D) after 808K is incubated 62min, 840K is warming up to 13min；
E) after 843K is incubated 42min, exit bonnet high wind and furnace body temperature is chilled to 355K, open firedoor handle nanocrystalline magnetic
Core takes out；
F) nanocrystalline magnet core taken out out of stove is placed on cooling frame again that high wind is chilled to normal temperature.
The step（4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
The nitrogen that the interior hydrogen and percent by volume that filled with mixed gas, mixed gas is 18% by percent by volume is 82% forms.
The step（5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again carries out impregnation and consolidated
Change is handled.
The step（6）In, impregnation curing process comprises the following steps：
A, nanocrystalline magnet core is preheated at a temperature of 68 DEG C；
B, epoxy resin shellac varnish is heated under 68 DEG C of environment of water-bath as curing agent using epoxy resin shellac varnish；And with dilution
Agent is using the ratio of shellac varnish and diluent as 1.1:1 dilutes to dissolve, and the shellac varnish after dilution is incubated 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, is impregnated with 45min,
Vacuum is 0.75Mpa；
D, the nanocrystalline magnet core after impregnation is solidified using three sections of thermal-insulating methods, 75 DEG C of first paragraph temperature, is incubated 70min；Second segment
115 DEG C of temperature, it is incubated 110min；3rd section of 155 DEG C of temperature, it is incubated 110min；Natural cooling.
Embodiment 5
A kind of iron nickel base nanometer crystalline substance magnetic core, the iron nickel base nanometer crystalline substance magnetic core are made up of iron-nickel alloy, and the iron nickel base nanometer is brilliant
Band includes the element of following percentage by weight：Ni：25%、Si：12%、B：5%、Nb：4%、Cu：0.5%、Co：8%, surplus Fe.
The iron nickel base nanometer crystal zone material also includes 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 nickel base nanometer crystalline substance magnetic core, comprises the following steps：
（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；
（3）Iron nickel base nanometer crystal zone material 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.
The step（3）In, the thickness of iron nickel base nanometer crystal zone material is 25 μm, width 30mm.
The step（4）With the step（5）In, it is the step of heat treatment：
A) 130min is passed through in-furnace temperature from room temperature to 660K；
B) after 663K is incubated 25min, 770K is warming up to 40min；
C) after 773K is incubated 45min, 810K is warming up to 15min；
D) after 813K is incubated 65min, 845K is warming up to 14min；
E) after 848K is incubated 45min, exit bonnet high wind and furnace body temperature is chilled to 360K, open firedoor handle nanocrystalline magnetic
Core takes out；
F) nanocrystalline magnet core taken out out of stove is placed on cooling frame again that high wind is chilled to normal temperature.
The step（4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, vacuum annealing furnace
The nitrogen that the interior hydrogen and percent by volume that filled with mixed gas, mixed gas is 20% by percent by volume is 80% forms.
The step（5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again carries out impregnation and consolidated
Change is handled.
The step（6）In, impregnation curing process comprises the following steps：
A, nanocrystalline magnet core is preheated at a temperature of 70 DEG C；
B, epoxy resin shellac varnish is heated under 70 DEG C of environment of water-bath as curing agent using epoxy resin shellac varnish；And with dilution
Agent is using the ratio of shellac varnish and diluent as 1.2:1 dilutes to dissolve, and the shellac varnish after dilution is incubated 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, is impregnated with 50min,
Vacuum is 0.8Mpa；
D, the nanocrystalline magnet core after impregnation is solidified using three sections of thermal-insulating methods, 80 DEG C of first paragraph temperature, is incubated 80min；Second segment
120 DEG C of temperature, it is incubated 120min；3rd section of 160 DEG C of temperature, it is incubated 120min；Natural cooling.
After tested, the Effective permeability μ e of nanocrystalline magnet core produced by the present invention can reach 9.1 × 104More than, saturation
Magnetic induction value Bs can reach more than 1.50T, and coercivity magnetic field intensity Hc value is less than 2Am-1, remanence ratio is less than 0.1, anti-direct current
Biasing ability is strong, and under 100Oe field strength, magnetic conductivity still has more than 80%, wherein loss value is under the conditions of 0.2T, 20k Hz
Below 1.2W/kg, while magnetic core loss value under the conditions of 0.5T, 20k Hz is below 5.6W/kg, magnetic core is in 0.5T, 50k Hz
Under the conditions of loss value be below 16.8W/kg.
The iron nickel base nanometer crystalline substance magnetic core of the present invention has stable magnetic conductivity and direct current biasing ability, also with high saturation magnetic
The advantages that induction, 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, the present invention can be realized with other manner,
Do not depart from and any on the premise of present inventive concept obviously replace within protection scope of the present invention.
Claims (10)
- A kind of 1. iron nickel base nanometer crystalline substance magnetic core, it is characterised in that：The iron nickel base nanometer crystalline substance magnetic core is made up of iron-nickel alloy, described Iron nickel base nanometer crystal zone material includes the element of following percentage by weight：Ni：15%-25%、Si：10%-12%、B：3%-5%、Nb：2%- 4%、Cu：0.3%-0.5%、Co：4%-8%, surplus Fe.
- A kind of 2. iron nickel base nanometer crystalline substance magnetic core according to claim 1, it is characterised in that：The iron nickel base nanometer crystal zone material Also include Ga：0.4%-0.8%、V：0.1%-0.5% and Ti：0.2%-0.6%.
- A kind of 3. iron nickel base nanometer crystalline substance magnetic core according to claim 1, it is characterised in that：The iron nickel base nanometer crystal zone material Also include Mn：1%-3%、Cr：0.5%-1.5% and Mo：0.8%-1.2%.
- A kind of 4. iron nickel base nanometer crystalline substance magnetic core according to claim 1, it is characterised in that：The iron nickel base nanometer crystal zone material Also include C：1.2%-1.4%、Ge：0.01%-0.05% and P：0.001%-0.005%.
- A kind of 5. iron nickel base nanometer crystalline substance magnetic core according to claim 1, it is characterised in that：The iron nickel base nanometer crystal zone material Also include Vb：1.4%-1.8%、Ta：0.3%-0.7% and W：0.04%-0.08%.
- A kind of 6. preparation method of iron nickel base nanometer crystalline substance magnetic core as described in claim any one of 1-5, it is characterised in that：Including Following steps：（1）The iron nickel base nanometer crystal zone material 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 nickel base nanometer crystal zone material；（3）Iron nickel base nanometer crystal zone material 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.
- A kind of 7. preparation method of iron nickel base nanometer crystalline substance magnetic core according to claim 6, it is characterised in that：The step （3）In, the thickness of iron nickel base nanometer crystal zone material is 15-25 μm, width 20-30mm.
- A kind of 8. preparation method of iron nickel base nanometer crystalline substance magnetic core according to claim 6, it is characterised in that：The step （4）With the step（5）In, it is the step of heat treatment：By 110-130min in-furnace temperature from room temperature to 640-660K；After 643-663K is incubated 15-25min, 750-770K is warming up to 32-40min；After 753-773K is incubated 35-45min, 790-810K is warming up to 11-15min；After 793-813K is incubated 55-65min, 825-845K is warming up to 10-14min；After 828-848K is incubated 35-45min, exits bonnet high wind and furnace body temperature is chilled to 340-360K, open firedoor handle Nanocrystalline magnet core takes out；The nanocrystalline magnet core taken out out of stove is placed on cooling frame again high wind is chilled to normal temperature.
- A kind of 9. preparation method of iron nickel base nanometer crystalline substance magnetic core according to claim 6, it is characterised in that：The step （4）With the step（5）In, the vacuum in vacuum annealing furnace is less than -0.1Mpa, filled with mixed gas in vacuum annealing furnace, The nitrogen that the hydrogen and percent by volume that mixed gas is 10%-20% by percent by volume are 80%-90% forms.
- A kind of 10. preparation method of iron nickel base nanometer crystalline substance magnetic core according to claim 6, it is characterised in that：The step （5）Also include step afterwards（6）Nanocrystalline magnet core after being heat-treated again carries out impregnation curing process.
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