CN107393672B - Iron-nickel-based nanocrystalline magnetic core and preparation method thereof - Google Patents
Iron-nickel-based nanocrystalline magnetic core and preparation method thereof Download PDFInfo
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- CN107393672B CN107393672B CN201710480272.XA CN201710480272A CN107393672B CN 107393672 B CN107393672 B CN 107393672B CN 201710480272 A CN201710480272 A CN 201710480272A CN 107393672 B CN107393672 B CN 107393672B
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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)
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Abstract
The invention relates to the technical field of high-frequency inverter power supplies, in particular to an iron-nickel-based nanocrystalline magnetic core and a preparation method thereof, wherein the iron-nickel-based nanocrystalline magnetic core is made of iron-nickel alloy, and the iron-nickel-based nanocrystalline strip comprises the following elements in percentage by weight: ni: 15% -25%, Si: 10% -12%, B: 3% -5%, Nb: 2% -4%, Cu: 0.3% -0.5%, Co: 4 to 8 percent of Fe, and the balance of Fe. The iron-nickel-based nanocrystalline magnetic core has stable magnetic conductivity and direct current bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance and the like, and has excellent comprehensive performance.
Description
Technical Field
The invention relates to the technical field of high-frequency inverter power supplies, in particular to an iron-nickel-based nanocrystalline magnetic core and a preparation method thereof.
Background
Soft magnetic materials are magnetic materials having low coercive force and high magnetic permeability, and are easy to magnetize and demagnetize, so that they are widely used in electrical and electronic devices. The iron-based amorphous alloy is used as a commonly used iron core soft magnetic material at present, mainly comprises Fe element, Si and B metal elements, has the characteristics of high saturation magnetic induction intensity, high magnetic conductivity, low iron core loss and the like, and can be widely applied to distribution transformers, high-power switching power supplies, pulse transformers, magnetic amplifiers, medium-frequency transformers and inverter iron cores.
The patent application with the application number of CN103258612A discloses a low-permeability magnetic core and a manufacturing method and application thereof, wherein the magnetic core is made of an iron-based amorphous material, the magnetic permeability is 500-5000, and the value of the coercive force magnetic field intensity is less than 10Am-1The annealing temperature for preparing the magnetic core material is 350-500 ℃, and the annealing time is within 2 h. The magnetostriction coefficient of the magnetic core of the iron-based amorphous material is high, and meanwhile, the annealing temperature during preparation is low, and the annealing time is short, so that the stress removal heat treatment is insufficient, further the stress is not completely eliminated, and the linearity of the magnetic conductivity of the permanent magnet is influenced; in addition, the magnetic core has low magnetic permeability and high soft magnetic property such as coercive force, so that the iron core has high loss and is not suitable for use in high-frequency and high-inductance use environments.
With the development of new electronic industry, more and higher requirements are provided for soft magnetic materials, such as the development of inverter power supplies of photovoltaic power, wind power, variable frequency dragging and the like, and the requirements of high inductance, high anti-saturation performance, excellent MHz-level frequency characteristic and the like are provided for the inductance of key components of electromagnetic compatibility, so that the iron-based nanocrystalline alloy is produced on the basis of iron-based amorphous materials. The alloy is mainly made of iron element, and a small amount of Nb, Cu, Si, B and other elements are added. The alloy formed by the elements can firstly form an amorphous material through a rapid solidification process, the amorphous material can obtain a nanocrystal main phase with the diameter of 10-20 nm after crystallization heat treatment, and meanwhile, a small amount of amorphous residual phase is also reserved, and the amorphous residual phase is generally referred to as the nanocrystal material for short. The nanocrystalline material has comprehensive magnetic properties such as high saturation magnetic induction, high initial permeability, low coercive force and the like, the magnetic core made of the nanocrystalline material has very low iron core loss under high frequency and high magnetic induction, and has extremely small magnetostriction coefficient and extremely strong induced anisotropy constant Ku, after longitudinal or transverse magnetic field treatment, the magnetic core with high residual magnetic induction intensity value or low residual magnetic induction intensity value can be obtained, and the nanocrystalline material can be widely applied to different frequency ranges. The nanocrystalline magnetic core is widely applied to high-power switching power supplies, inverter power supplies, magnetic amplifiers, high-frequency transformers, high-frequency converters, high-frequency choke coil iron cores, current transformer iron cores, leakage protection switches and common-mode inductance iron cores.
The existing magnetic core products mainly comprise an iron core, an iron-silicon-aluminum magnetic core, an iron-nickel magnetic core, an MPP magnetic core and the like. The conventional iron-nickel magnetic core has excellent frequency characteristics in the frequency range of 1MHz, low loss, highest direct current bias capability and good product performance. However, the iron-nickel magnetic core contains 50% of nickel, so the price is high and the production cost is high.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the iron-nickel-based nanocrystalline magnetic core which has stable magnetic conductivity and direct current bias capability, has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance and the like, and has excellent comprehensive performance.
The invention also aims to provide a preparation method of the iron-nickel-based nanocrystalline magnetic core, which has the advantages of simple process, convenient operation and control, stable quality, high production efficiency and low production cost and can be used for large-scale industrial production.
The purpose of the invention is realized by the following technical scheme: an iron-nickel based nanocrystalline magnetic core made of an iron-nickel alloy, the iron-nickel based nanocrystalline strip comprising the following elements in weight percent: ni: 15% -25%, Si: 10% -12%, B: 3% -5%, Nb: 2% -4%, Cu: 0.3% -0.5%, Co: 4 to 8 percent of Fe, and the balance of Fe.
The amorphous forming elements Si and B, iron-based nanocrystalline soft magnetic alloy are generally based on amorphous alloy, and form nanocrystalline material through proper crystallization annealing, so that the amorphous element is a basic component element, particularly the B element, the atomic radius of the B element is smaller, the outer layer electrons are more, the amorphous alloy is very favorable for forming, and Si is also an important amorphous element;
the nanocrystalline forms elements Cu and Nb, Cu is firstly separated from Fe during crystallization to form an enrichment area of the metal element, the enrichment area plays a nucleation role for the nanocrystallization, the Nb element is slowly diffused and mainly acts to block the growth of α -Fe crystal grains, so that the crystal grain size is ensured to be in a nanometer level, and the control of the Cu and Nb contents is very important for keeping the microstructure of the magnetic core.
The addition of Cu element can form high-density α -phase crystal nuclei at the initial stage of the subsequent amorphous crystallization to serve as growth centers of nano-sized crystals.
The iron-nickel-based nanocrystalline magnetic core is improved on the basis of the formula of the traditional iron-based nanocrystalline magnetic core, the metal nickel is added in a proper proportion, and the prepared nanocrystalline magnetic core has better toughness, temperature resistance and magnetic permeability.
The Fe-Ni based nanocrystalline magnetic core of the invention replaces part of Fe with Co element, can obviously improve the high temperature, high frequency characteristic and quality factor of the magnetic core, and the Curie temperature and the magnetization intensity of the magnetic core are obviously improved compared with that before Fe is replaced by Co.
The iron-nickel-based nanocrystalline magnetic core provided by the invention adopts Al and Ni to partially replace noble metal Nb in the magnetic core, the addition of Nb is favorable for improving the saturation magnetic induction strength of the magnetic core, the addition of Al is favorable for reducing the coercive force, and meanwhile, the production cost of the magnetic core can be obviously reduced.
By adopting the elements and strictly controlling the weight percentage of each raw material, the iron-nickel-based nanocrystalline magnetic core prepared by the method has stable magnetic conductivity and direct current bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance and the like, and has excellent comprehensive performance.
Preferably, the iron-nickel based nanocrystalline strip further comprises Ga: 0.4% -0.8%, V: 0.1% -0.5% and Ti: 0.2 to 0.6 percent.
The Fe-Ni based nanocrystalline strip can improve the first crystallization temperature of the alloy by increasing Ga, V and Ti elements and strictly controlling the weight percentage of each raw material, thereby reducing the difference between the two crystallization temperatures.
Preferably, the iron-nickel based nanocrystalline strip further comprises Mn: 1% -3%, Cr: 0.5% -1.5% and Mo: 0.8 to 1.2 percent.
According to the iron-nickel-based nanocrystalline strip, the Mn, Cr and Mo elements are added, and the weight percentage of each raw material is strictly controlled, so that the material can form a strong annealing induced anisotropy constant, and a controllable and adjustable transverse magnetic anisotropy is formed in the transverse magnetic annealing process, so that the linear magnetic permeability and the anti-saturation characteristic are achieved.
Preferably, the iron-nickel based nanocrystalline strip further comprises C: 1.2% -1.4%, Ge: 0.01% -0.05% and P: 0.001% -0.005%.
The iron-nickel-based nanocrystalline strip can improve the first crystallization temperature of the alloy by adding C, Ge and P elements and strictly controlling the weight percentage of each raw material, thereby reducing the difference between the two crystallization temperatures.
Preferably, the iron-nickel based nanocrystalline strip further comprises Vb: 1.4% -1.8%, Ta: 0.3% -0.7% and W: 0.04 to 0.08 percent.
The iron-nickel-based nanocrystalline strip can prevent nanocrystalline grains from growing by adding Vb, Ta and W elements and strictly controlling the weight percentage of each raw material, and maintain and finally form a nanoscale crystal size structure.
A preparation method of an iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) and putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again.
Preferably, in the step (3), the thickness of the iron-nickel based nanocrystalline strip is 15-25 μm, and the width is 20-30 mm. According to the invention, the thickness and the width of the iron-nickel-based nanocrystalline strip are strictly controlled, so that the loss value of the product is reduced and the direct current bias capability is improved while the iron-nickel-based nanocrystalline magnetic core keeps good inductance and higher quality factor.
Preferably, in the step (4) and the step (5), the heat treatment step is:
a) the temperature in the furnace is raised from room temperature to 640-660K after 110-130 min;
b) after heat preservation is carried out for 15-25min at 643-663K, the temperature is raised to 750-770K within 32-40 min;
c) after the temperature is kept for 35-45min at 753-773K, the temperature is raised to 790-810K within 11-15 min;
d) after the temperature is kept for 55-65min at 793-813K, the temperature is raised to 825-845K for 10-14 min;
e) after the temperature is kept for 35-45min at 828-;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
The annealing process of the invention uses the conventional lattice annealing furnace to carry out the same heat treatment process twice on the nanocrystalline magnetic core to be subjected to heat treatment so as to meet the requirement of the transverse magnetic furnace on reducing the electrical property of the nanocrystalline magnetic core Br, thereby simplifying the heat treatment process, having simple process, reducing the investment of production equipment, saving the electric power cost by more than 25 percent and having low production cost. The nanocrystalline magnetic core prepared by the annealing process has stable magnetic conductivity and direct current bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance and the like, and has excellent comprehensive performance.
Preferably, in the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, the vacuum annealing furnace is filled with mixed gas, and the mixed gas consists of 10-20% by volume of hydrogen and 80-90% by volume of nitrogen.
The invention can improve the magnetic conductivity of the nanocrystalline magnetic core by strictly controlling the vacuum degree in the vacuum annealing furnace and filling the nitrogen-hydrogen mixed gas in the vacuum annealing furnace. After nitrogen is injected, the nitrogen mainly plays a role of uniform temperature, the nitrogen is a heat conduction medium, so that the magnetic core in the furnace is uniformly heated, the temperature of the magnetic core is uniform and balanced, the magnetic conductivity of the nanocrystalline magnetic core is related to the atmosphere of the annealing furnace, and the magnetic conductivity has certain difference when the atmosphere of the annealing furnace is different; the following conclusion is obtained through experiments, and the magnetic permeability change rule of the magnetic core is as follows: the vacuum-pumping in the annealing furnace is better than that before the vacuum-pumping; the vacuumizing is better than the vacuumizing only, and the nitrogen-hydrogen mixed gas is filled in the vacuumizing.
Preferably, the step (5) is followed by a step (6) of performing a dipping and curing treatment on the nanocrystalline magnetic core after the heat treatment is performed again.
In the step (6), the gum dipping and curing treatment comprises the following steps:
A. preheating the nanocrystalline magnetic core at the temperature of 60-70 ℃;
B. heating the epoxy resin adhesive paint in a water bath at 60-70 ℃ by taking the epoxy resin adhesive paint as a curing agent; mixing and diluting with diluent at a ratio of glue paint to diluent of 0.8-1.2:1, and keeping the diluted glue paint at 60-70 deg.C for 40-80 min;
C. soaking the preheated nanocrystalline magnetic core in the blended hot glue paint in a vacuum impregnation mode for 30-50min, wherein the vacuum degree is 0.6-0.8 Mpa;
D. curing the impregnated nanocrystalline magnetic core by a three-stage heat preservation method, wherein the temperature of the first stage is 60-80 ℃, and preserving heat for 40-80 min; the temperature of the second section is 100 ℃ and 120 ℃, and the temperature is kept for 80-120 min; the temperature of the third section is 140 ℃ and 160 ℃, and the temperature is kept for 80-120 min; and (5) naturally cooling.
In order to solve the problem of the curing mode of the nanocrystalline magnetic core, the curing step of the method adopts glue with high bonding strength and low stress to cure and form, namely epoxy resin glue paint. Pre-heating glue lacquer and nanocrystalline magnetic core before soaking for temperature between them all keeps 60-70 ℃, and when epoxy glue lacquer was about 70 ℃, the activity increased, and viscosity can descend, just so can guarantee drenching when gluing, unnecessary glue lacquer can be through the inside of the nanocrystalline magnetic core of self action of gravity outflow, guaranteed that the surface of nanocrystalline magnetic core is clean, does not influence the subsequent cutting precision of magnetic core. Secondly, in order to further improve the viscosity and the fluidity of the glue paint after heating, acetone is used as a diluent, and the glue paint and the diluent are mixed according to the proportion of 0.8-1.2: 1. And after impregnation, a three-section heat preservation method is adopted for solidification, so that the mixed glue paint forms a sealing film on the surface of the nanocrystalline magnetic core under the condition of high temperature, the glue paint is ensured to be remained in the nanocrystalline magnetic core, the problems of paint leakage, low strength and the like in the conventional mode are solved, and meanwhile, the high strength and low stress of the glue paint play a role in assisting the final cutting of the product without damage and the mirror surface requirement.
The invention has the beneficial effects that: the iron-nickel-based nanocrystalline magnetic core has stable magnetic conductivity and direct current bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance and the like, and has excellent comprehensive performance.
The preparation method has the advantages of simple process, convenient operation and control, stable quality, high production efficiency and low production cost, and can be used for large-scale industrial production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
An iron-nickel based nanocrystalline magnetic core made of an iron-nickel alloy, the iron-nickel based nanocrystalline strip comprising the following elements in weight percent: ni: 15%, Si: 10%, B: 3%, Nb: 2%, Cu: 0.3%, Co: 4 percent and the balance of Fe.
The iron-nickel based nanocrystalline strip further comprises 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 percent.
A preparation method of an iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) and putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again.
In the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 15 μm, and the width of the iron-nickel-based nanocrystalline strip is 20 mm.
In the step (4) and the step (5), the heat treatment step is:
a) heating the temperature in the furnace from room temperature to 640K after 110 min;
b) after 643K is kept for 15min, the temperature is raised to 750K within 32 min;
c) keeping the temperature at 753K for 35min, and heating to 790K in 11 min;
d) after the temperature is kept at 793K for 55min, the temperature is increased to 825K within 10 min;
e) after the temperature is kept for 35min at 828K, the furnace cover is withdrawn and strong wind is blown out to rapidly cool the temperature of the furnace body to 340K, and a furnace door is opened to take out the nanocrystalline magnetic core;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, mixed gas is filled in the vacuum annealing furnace, and the mixed gas consists of 10% by volume of hydrogen and 90% by volume of nitrogen.
And (5) after the step (6), performing gum dipping and curing treatment on the nanocrystalline magnetic core subjected to heat treatment again.
In the step (6), the gum dipping and curing treatment comprises the following steps:
A. preheating the nanocrystalline magnetic core at the temperature of 60 ℃;
B. heating the epoxy resin adhesive paint in a water bath at 60 ℃ by using the epoxy resin adhesive paint as a curing agent; blending and diluting with a diluent according to the ratio of the glue paint to the diluent of 0.8:1, and keeping the temperature of the diluted glue paint at 60 ℃ for 40 min;
C. soaking the preheated nanocrystalline magnetic core in the blended hot glue paint in a vacuum impregnation mode for 30min, wherein the vacuum degree is 0.6 Mpa;
D. curing the impregnated nanocrystalline magnetic core by a three-stage heat preservation method, wherein the temperature of the first stage is 60 ℃, and preserving heat for 40 min; the temperature of the second stage is 100 ℃, and the temperature is kept for 80 min; the temperature of the third section is 140 ℃, and the temperature is kept for 80 min; and (5) naturally cooling.
Example 2
An iron-nickel based nanocrystalline magnetic core made of an iron-nickel alloy, the iron-nickel based nanocrystalline strip comprising the following elements in weight percent: ni: 18%, Si: 11.5%, B: 3.5%, Nb: 2.5%, Cu: 0.35%, Co: 5 percent, and the balance being Fe.
The iron-nickel based nanocrystalline strip further comprises 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 percent.
A preparation method of an iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) and putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again.
In the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 15-25 μm, and the width is 20-30 mm.
In the step (4) and the step (5), the heat treatment step is:
a) heating the temperature in the furnace from room temperature to 645K after 115 min;
b) after heat preservation at 648K for 18min, heating to 755K in 34 min;
c) after the temperature is kept for 758K and 38min, the temperature is increased to 795K within 12 min;
d) after the temperature is kept at 798K for 58min, the temperature is increased to 830K within 11 min;
e) after the temperature is kept at 833K for 38min, the furnace cover is withdrawn and strong wind is blown to rapidly cool the furnace body to 345K, and a furnace door is opened to take out the nanocrystalline magnetic core;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, mixed gas is filled in the vacuum annealing furnace, and the mixed gas consists of 12% by volume of hydrogen and 88% by volume of nitrogen.
And (5) after the step (6), performing gum dipping and curing treatment on the nanocrystalline magnetic core subjected to heat treatment again.
In the step (6), the gum dipping and curing treatment comprises the following steps:
A. preheating the nanocrystalline magnetic core at the temperature of 62 ℃;
B. heating the epoxy resin adhesive paint in a water bath at 62 ℃ by using the epoxy resin adhesive paint as a curing agent; blending and diluting with a diluent according to the ratio of the glue paint to the diluent of 0.9:1, and keeping the temperature of the diluted glue paint at 62 ℃ for 50 min;
C. soaking the preheated nanocrystalline magnetic core in blended hot glue paint in a vacuum impregnation mode for 35min, wherein the vacuum degree is 0.65 Mpa;
D. curing the impregnated nanocrystalline magnetic core by a three-stage heat preservation method, wherein the first stage temperature is 65 ℃, and preserving heat for 50 min; the temperature of the second stage is 105 ℃, and the temperature is kept for 90 min; the temperature of the third section is 145 ℃, and the temperature is kept for 90 min; and (5) naturally cooling.
Example 3
An iron-nickel based nanocrystalline magnetic core made of an iron-nickel alloy, the iron-nickel based nanocrystalline strip comprising the following elements in weight percent: ni: 20%, Si: 11%, B: 4%, Nb: 3%, Cu: 0.4%, Co: 6 percent and the balance of Fe.
The iron-nickel based nanocrystalline strip further comprises 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 percent.
A preparation method of an iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) and putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again.
In the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 20 μm, and the width is 25 mm.
In the step (4) and the step (5), the heat treatment step is:
a) heating the temperature in the furnace from room temperature to 650K after 120 min;
b) after maintaining the temperature at 653K for 20min, heating to 760K within 36 min;
c) keeping the temperature at 763K for 40min, and heating to 800K for 13 min;
d) after the temperature is preserved for 60min at 803K, the temperature is raised to 835K within 12 min;
e) after the temperature is kept for 40min at 838K, the furnace cover is withdrawn and strong wind is blown out to rapidly cool the temperature of the furnace body to 350K, and a furnace door is opened to take out the nanocrystalline magnetic core;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, mixed gas is filled in the vacuum annealing furnace, and the mixed gas consists of 15% by volume of hydrogen and 85% by volume of nitrogen.
And (5) after the step (6), performing gum dipping and curing treatment on the nanocrystalline magnetic core subjected to heat treatment again.
In the step (6), the gum dipping and curing treatment comprises the following steps:
A. preheating the nanocrystalline magnetic core at 65 ℃;
B. heating the epoxy resin adhesive paint in a water bath at 65 ℃ by using the epoxy resin adhesive paint as a curing agent; blending and diluting the mixed paint with a diluent according to the ratio of 1:1, and keeping the diluted paint at 65 ℃ for 60 min;
C. soaking the preheated nanocrystalline magnetic core in the blended hot glue paint in a vacuum impregnation mode for 40min, wherein the vacuum degree is 0.7 Mpa;
D. curing the impregnated nanocrystalline magnetic core by a three-stage heat preservation method, wherein the first stage temperature is 70 ℃, and preserving heat for 60 min; the temperature of the second stage is 110 ℃, and the temperature is kept for 810 min; the temperature of the third section is 150 ℃, and the temperature is kept for 100 min; and (5) naturally cooling.
Example 4
An iron-nickel based nanocrystalline magnetic core made of an iron-nickel alloy, the iron-nickel based nanocrystalline strip comprising the following elements in weight percent: ni: 22%, Si: 11.5%, B: 4.5%, Nb: 3.5%, Cu: 0.45%, Co: 7 percent and the balance of Fe.
The iron-nickel based nanocrystalline strip further comprises 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 percent.
A preparation method of an iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) and putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again.
In the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 22 μm, and the width of the iron-nickel-based nanocrystalline strip is 28 mm.
In the step (4) and the step (5), the heat treatment step is:
a) raising the temperature in the furnace from room temperature to 655K after 125 min;
b) after preserving heat for 22min at 658K, heating to 765K in 38 min;
c) after the temperature is kept for 42min at 768K, the temperature is increased to 805K within 14 min;
d) after the temperature is kept for 62min at 808K, the temperature is increased to 840K within 13 min;
e) after the temperature is kept for 42min at 843K, the furnace cover is withdrawn and strong wind is blown out to rapidly cool the furnace body to 355K, and a furnace door is opened to take out the nanocrystalline magnetic core;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, mixed gas is filled in the vacuum annealing furnace, and the mixed gas consists of 18% of hydrogen and 82% of nitrogen by volume percentage.
And (5) after the step (6), performing gum dipping and curing treatment on the nanocrystalline magnetic core subjected to heat treatment again.
In the step (6), the gum dipping and curing treatment comprises the following steps:
A. preheating the nanocrystalline magnetic core at 68 ℃;
B. heating the epoxy resin adhesive paint in a water bath at 68 ℃ by using the epoxy resin adhesive paint as a curing agent; blending and diluting with a diluent according to the ratio of the glue paint to the diluent of 1.1:1, and keeping the temperature of the diluted glue paint at 68 ℃ for 70 min;
C. soaking the preheated nanocrystalline magnetic core in blended hot glue paint in a vacuum impregnation mode for 45min, wherein the vacuum degree is 0.75 Mpa;
D. curing the impregnated nanocrystalline magnetic core by a three-stage heat preservation method, wherein the first stage temperature is 75 ℃, and preserving heat for 70 min; the second stage temperature is 115 ℃, and the temperature is kept for 110 min; the temperature of the third section is 155 ℃, and the temperature is kept for 110 min; and (5) naturally cooling.
Example 5
An iron-nickel based nanocrystalline magnetic core made of an iron-nickel alloy, the iron-nickel based nanocrystalline strip comprising the following elements in weight percent: ni: 25%, Si: 12%, B: 5%, Nb: 4%, Cu: 0.5%, Co: 8 percent and the balance of Fe.
The iron-nickel based nanocrystalline strip further comprises 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 percent.
A preparation method of an iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) and putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again.
In the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 25 μm, and the width is 30 mm.
In the step (4) and the step (5), the heat treatment step is:
a) heating the temperature in the furnace from room temperature to 660K after 130 min;
b) after the temperature is kept at 663K for 25min, the temperature is increased to 770K within 40 min;
c) keeping the temperature at 773K for 45min, and heating to 810K in 15 min;
d) after the temperature is kept at 813K for 65min, the temperature is increased to 845K in 14 min;
e) after the temperature is kept for 45min at 848K, the furnace cover is withdrawn and strong wind is blown out to rapidly cool the furnace body to 360K, and a furnace door is opened to take out the nanocrystalline magnetic core;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, mixed gas is filled in the vacuum annealing furnace, and the mixed gas consists of 20% of hydrogen and 80% of nitrogen by volume percentage.
And (5) after the step (6), performing gum dipping and curing treatment on the nanocrystalline magnetic core subjected to heat treatment again.
In the step (6), the gum dipping and curing treatment comprises the following steps:
A. preheating the nanocrystalline magnetic core at the temperature of 70 ℃;
B. heating the epoxy resin adhesive paint in a water bath at 70 ℃ by using the epoxy resin adhesive paint as a curing agent; blending and diluting with a diluent according to the ratio of the glue paint to the diluent of 1.2:1, and keeping the temperature of the diluted glue paint at 70 ℃ for 80 min;
C. soaking the preheated nanocrystalline magnetic core in blended hot glue paint in a vacuum impregnation mode for 50min, wherein the vacuum degree is 0.8 Mpa;
D. curing the impregnated nanocrystalline magnetic core by a three-stage heat preservation method, wherein the first stage temperature is 80 ℃, and preserving heat for 80 min; the temperature of the second stage is 120 ℃, and the temperature is kept for 120 min; the temperature of the third section is 160 ℃, and the temperature is kept for 120 min; and (5) naturally cooling.
Tests prove that the effective magnetic permeability mu e of the nanocrystalline magnetic core prepared by the invention can reach 9.1 multiplied by 104Above, the saturation magnetic induction value Bs can reach more than 1.50T, and the value of the coercive force magnetic field strength Hc is less than 2Am-1The remanence ratio is less than 0.1, the DC bias resistance is strong, the magnetic conductivity is still more than 80% under the field intensity of 100Oe, wherein the loss value is less than 1.2W/kg under the conditions of 0.2T and 20k Hz, the loss value of the magnetic core is less than 5.6W/kg under the conditions of 0.5T and 20k Hz, and the loss value of the magnetic core is less than 16.8W/kg under the conditions of 0.5T and 50k Hz.
The iron-nickel-based nanocrystalline magnetic core has stable magnetic conductivity and direct current bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance and the like, and has excellent comprehensive performance.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (4)
1. An iron-nickel based nanocrystalline magnetic core, characterized in that: the iron-nickel-based nanocrystalline magnetic core is made of iron-nickel alloy, and comprises the following elements in percentage by weight: ni: 15% -25%, Si: 10% -12%, B: 3% -5%, Nb: 2% -4%, Cu: 0.3% -0.5%, Co: 4% -8%, the balance being Fe, and also comprising Ga: 0.4% -0.8%, V:
0.1% -0.5% and Ti: 0.2% -0.6%, further comprising Mn: 1% -3%, Cr: 0.5% -1.5% and Mo: 0.8% -1.2%, further comprising C: 1.2% -1.4%, Ge: 0.01% -0.05% and P: 0.001% -0.005%;
the preparation method of the iron-nickel-based nanocrystalline magnetic core comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again;
in the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 15-25 μm, and the width is 20-30 mm;
in the step (4) and the step (5), the heat treatment step is:
a) the temperature in the furnace is raised from room temperature to 640-660K after 110-130 min;
b) after heat preservation is carried out for 15-25min at 643-663K, the temperature is raised to 750-770K within 32-40 min;
c) after the temperature is kept for 35-45min at 753-773K, the temperature is raised to 790-810K within 11-15 min;
d) after the temperature is kept for 55-65min at 793-813K, the temperature is raised to 825-845K for 10-14 min;
e) after the temperature is kept for 35-45min at 828-;
f) and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
2. The method of claim 1, wherein the iron-nickel based nanocrystalline core comprises: the method comprises the following steps:
(1) smelting the iron-nickel-based nanocrystalline strip raw material to obtain an alloy melt;
(2) spraying the alloy melt by adopting a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
(3) winding the iron-nickel-based nanocrystalline strip into an annular nanocrystalline magnetic core;
(4) putting the nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment;
(5) putting the nanocrystalline magnetic core after heat treatment into a vacuum annealing furnace for heat treatment again;
in the step (3), the thickness of the iron-nickel-based nanocrystalline strip is 15-25 μm, and the width is 20-30 mm;
in the step (4) and the step (5), the heat treatment step is:
the temperature in the furnace is raised from room temperature to 640-660K after 110-130 min;
after heat preservation is carried out for 15-25min at 643-663K, the temperature is raised to 750-770K within 32-40 min;
after the temperature is kept for 35-45min at 753-773K, the temperature is raised to 790-810K within 11-15 min;
after the temperature is kept for 55-65min at 793-813K, the temperature is raised to 825-845K for 10-14 min;
after the temperature is kept for 35-45min at 828-;
and placing the nanocrystalline magnetic core taken out of the furnace on a cooling frame, and rapidly cooling to normal temperature by strong wind.
3. The method of claim 2, wherein the iron-nickel based nanocrystalline magnetic core comprises: in the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than-0.1 Mpa, mixed gas is filled in the vacuum annealing furnace, and the mixed gas consists of 10-20% of hydrogen and 80-90% of nitrogen by volume percentage.
4. The method of claim 2, wherein the iron-nickel based nanocrystalline magnetic core comprises: and (5) after the step (6), performing gum dipping and curing treatment on the nanocrystalline magnetic core subjected to heat treatment again.
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