CN107345265B - A kind of annealing process for the remanent magnetism reducing nanocrystalline magnet core - Google Patents
A kind of annealing process for the remanent magnetism reducing nanocrystalline magnet core Download PDFInfo
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- CN107345265B CN107345265B CN201710479921.4A CN201710479921A CN107345265B CN 107345265 B CN107345265 B CN 107345265B CN 201710479921 A CN201710479921 A CN 201710479921A CN 107345265 B CN107345265 B CN 107345265B
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Abstract
The present invention relates to high frequency inverter technical fields, and in particular to a kind of annealing process for the remanent magnetism for reducing nanocrystalline magnet core includes the following steps: that nanocrystalline strip is wound into circular nano crystalline substance magnetic core by (1).(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.The conventional lattice annealing furnace of annealing process of the invention reaches the nanocrystalline magnet core to be heat-treated by identical heat treatment process twice the electrical requirements of horizontal magnetic furnace reduction nanocrystalline magnet core remanent magnetism, simplify heat treatment process, simple process, reduce production equipment investment, 25% or more power cost can also be saved, production cost is low.Nanocrystalline magnet core made from annealing process through 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 annealing for the remanent magnetism for reducing nanocrystalline magnet core
Technique.
Background technique
Soft magnetic materials has the magnetic characteristics such as low-coercivity, high magnetic permeability, is production inductor, choke coil, sensor equimagnetic
The raw material of core are used widely in industries such as electric power, motor and electronics at present.So far, for engineer application
Soft magnetic materials, because its soft magnetic characteristic and using power, frequency different condition due to be divided into metal soft magnetic material (such as ingot iron,
Silicon steel, permalloy), soft magnetic ferrite, amorphous and nano crystal soft magnetic material.The coercivity of traditional metal soft magnetic material is opposite
It is higher, it is limited in the application in soft magnetism field；Soft magnetic ferrite is unfavorable for electronic component because saturation induction density is lower
Miniaturization；And brand-new material of the nanometer crystal alloy soft magnetic materials as this field, because having high-saturation magnetic induction strong simultaneously
The advantages that degree, high magnetic permeability, low-loss (being far below silicon steel), high resistivity and high-strength tenacity, numerous researchers are attracted
Note that just put into production application from research initial stage, and its preparation process is simple, energy conservation and environmental protection, in a small number of fields part
Instead of traditional silicon steel and Ferrite Material.
With the maturation that technology develops, nanocrystalline magnet core using more and more extensive, but will reduce this magnetic in inverter
The remanent magnetism of core, existing general annealing process are to add transverse magnetic to handle with horizontal magnetic furnace.
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 reduction is nanocrystalline
The annealing process of the remanent magnetism of magnetic core, annealing process routine lattice annealing furnace is the nanocrystalline magnet core to be heat-treated by twice
Identical heat treatment process is to reach the electrical requirements that horizontal magnetic furnace reduces nanocrystalline magnet core remanent magnetism, simple process, and production cost is low.
The purpose of the invention is achieved by the following technical solution: a kind of annealing process for the remanent magnetism reducing nanocrystalline magnet core,
Include the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
Preferably, in the step (1), nanocrystalline strip with a thickness of 15-25 μm, width 20-30mm.The present invention is logical
The thickness and width of strict control nanocrystalline strip is crossed, so that nanocrystalline magnet core is keeping good inductance, higher quality
While factor, the loss value of product is reduced, improves direct current biasing ability.
Preferably, in the step (1), nanocrystalline strip is iron based nano crystal band, the iron based nano crystal band packet
Include 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.
More preferably, the iron based nano crystal band further includes Ga:0.4%-0.8%, V:0.1%-0.5%, Ti:0.2%-
0.6%, Mn:1%-3%, Cr:0.5%-1.5%, Mo:0.8%-1.2%, C:1.2%-1.4%, Ge:0.01%-0.05%, P:0.001%-
0.005%, 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 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.It is of the invention iron-based to receive
Rice crystal zone material can be such that material is formed stronger by increasing Mn, Cr and Mo element, and the weight percent of each raw material of strict control
Annealing induced anisotropy constant, during horizontal magnetic anneal formed controllable adjustment lateral magnetic anisotropy, to reach line
The characteristic of property magnetic conductivity and anti-saturation.Iron based nano crystal band of the invention is by increasing C, Ge and P element, and strict control is each
The weight percent of raw material, can be improved the first time crystallization temperature of alloy, to reduce the gap between crystallization temperature twice.
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, can be with
It prevents nanocrystalline crystal grain from growing up, maintain and ultimately forms nanoscale crystalline size structure.
Another preferred, in the step (1), nanocrystalline strip is iron nickel base nanometer crystal zone material, the iron nickel base nanometer
Crystal zone material includes the element of following weight percent: 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 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.
Cu element, which is added, can crystallize nucleus in formation of subsequent Amorphous Crystallization initial stage high density α phase, to make
For the organic centre of nm-sized crystalline.
Iron nickel base nanometer crystalline substance magnetic core of the 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 magnetic permeability.
Replace part Fe with Co element in iron nickel base nanometer crystalline substance magnetic core of the invention, can significantly improve magnetic core high temperature,
High frequency characteristics and quality factor significantly improve before the Curie temperature of magnetic core, intensity of magnetization ratio Co replacement of fe.
Iron nickel base nanometer crystalline substance magnetic core of the invention replaces the noble metal Nb in magnetic core using the part Al, Ni, and addition Nb is advantageous
In the Saturation magnetic sense intensity for improving magnetic core, addition Al is conducive to coercitive reduction, while can be substantially reduced the production of magnetic core
Cost.
Iron nickel base nanometer crystal zone material of the invention is by using above-mentioned element, and the weight percent of each raw material of strict control
Than iron nickel base nanometer crystalline substance magnetic core obtained has stable magnetic conductivity and direct current biasing ability, also has high-saturation magnetic induction strong
The advantages that degree, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
More preferably, iron nickel base nanometer crystal zone material further includes Ga:0.4%-0.8%, V:0.1%-0.5%, Ti:
0.2%-0.6%, Mn:1%-3%, Cr:0.5%-1.5%, Mo:0.8%-1.2%, C:1.2%-1.4%, Ge:0.01%-0.05%, P:
0.001%-0.005%, Vb:1.4%-1.8%, Ta:0.3%-0.7% and W:0.04%-0.08%.
Iron nickel base nanometer crystal zone material of the invention is by increasing Ga, V and Ti element, and the weight hundred of each raw material of strict control
Divide ratio, the first time crystallization temperature of alloy can be improved, to reduce the gap between crystallization temperature twice.Iron nickel of the invention
Base nanometer crystal band can be such that material is formed by increasing Mn, Cr and Mo element, and the weight percent of each raw material of strict control
Stronger annealing induced anisotropy constant forms the lateral magnetic anisotropy of controllable adjustment, during horizontal magnetic anneal to reach
To the characteristic of linear magnetic conductivity and anti-saturation.Iron nickel base nanometer crystal zone material of the invention, which passes through, increases C, Ge and P element, and stringent
The weight percent for controlling each raw material, can be improved the first time crystallization temperature of alloy, thus between reducing crystallization temperature twice
Gap.Iron nickel base nanometer crystal zone material of the invention is by increasing Vb, Ta and W element, and the weight hundred of each raw material of strict control
Divide ratio, nanocrystalline crystal grain can be prevented to grow up, maintain and ultimately form nanoscale crystalline size structure.
Preferably, in the step (2) and the step (3), 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.
Annealing process of the invention leads to the nanocrystalline magnet core to be heat-treated with conventional lattice annealing furnace using repeatedly heat preservation
After identical heat treatment process twice to reach the electrical requirements that horizontal magnetic furnace reduces nanocrystalline magnet core remanent magnetism, heat treatment work is simplified
Skill, simple process reduce production equipment investment, can also save 25% or more power cost, production cost is low.
More preferably, in the step (2) and the step (3), 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.
Preferably, in the step (2) and the step (3), 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 (3) further includes that the nanocrystalline magnet core after step (4) will be heat-treated again carries out later
Impregnation curing process.
In the step (4), 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: the conventional lattice annealing furnace of annealing process of the invention is the nanometer to be heat-treated
Brilliant magnetic core reaches the electrical requirements of horizontal magnetic furnace reduction nanocrystalline magnet core remanent magnetism by identical heat treatment process twice, simplifies heat
Treatment process, simple process reduce production equipment investment, can also save 25% or more power cost, production cost is low.It is logical
Nanocrystalline magnet core made from annealing process of the invention is crossed with stable magnetic conductivity and direct current biasing ability, also there is high saturation
The advantages that magnetic induction intensity, low loss-value, low-coercivity, high temperature resistant, high comprehensive performance.
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 annealing process for the remanent magnetism reducing nanocrystalline magnet core, includes the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (1), nanocrystalline strip with a thickness of 15 μm, width 20mm.
In the step (1), nanocrystalline strip is iron based nano crystal band, and the iron based nano crystal band includes following weight
Measure the element of percentage: Si:14%, B:7%, Nb:1%, Cu:1.6%, Zr:4%, Al:0.5%, surplus 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%.
In the step (2) and the step (3), 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 (2) and the step (3), 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 (3) further includes that the nanocrystalline magnet core progress impregnation after step (4) will be heat-treated again is consolidated later
Change processing.
In the step (4), 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 annealing process for the remanent magnetism reducing nanocrystalline magnet core, includes the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (1), nanocrystalline strip with a thickness of 18 μm, width 22mm.
In the step (1), nanocrystalline strip is iron based nano crystal band, and the iron based nano crystal band includes following weight
Measure the element of percentage: 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%.
In the step (2) and the step (3), 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 (2) and the step (3), 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 (3) further includes that the nanocrystalline magnet core progress impregnation after step (4) will be heat-treated again is consolidated later
Change processing.
In the step (4), 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 annealing process for the remanent magnetism reducing nanocrystalline magnet core, includes the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (1), nanocrystalline strip with a thickness of 20 μm, width 25mm.
In the step (1), nanocrystalline strip is iron based nano crystal band, and the iron based nano crystal band includes following weight
Measure the element of percentage: Si:15%, B:8%, Nb:2%, Cu:1.7%, Zr:5%, Al:1.0%, surplus 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%.
In the step (2) and the step (3), 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 (2) and the step (3), 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 (3) further includes that the nanocrystalline magnet core progress impregnation after step (4) will be heat-treated again is consolidated later
Change processing.
In the step (4), 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 annealing process for the remanent magnetism reducing nanocrystalline magnet core, includes the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (1), nanocrystalline strip with a thickness of 22 μm, width 28mm.
In the step (1), nanocrystalline strip is iron based nano crystal band, and the iron based nano crystal band includes following weight
Measure the element of percentage: 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%.
In the step (2) and the step (3), 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 (2) and the step (3), 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 (3) further includes that the nanocrystalline magnet core progress impregnation after step (4) will be heat-treated again is consolidated later
Change processing.
In the step (4), 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 annealing process for the remanent magnetism reducing nanocrystalline magnet core, includes the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again.
In the step (1), nanocrystalline strip with a thickness of 25 μm, width 30mm.
In the step (1), nanocrystalline strip is iron based nano crystal band, and the iron based nano crystal band includes following weight
Measure the element of percentage: Si:16%, B:9%, Nb:3%, Cu:1.8%, Zr:6%, Al:1.5%, surplus 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%.
In the step (2) and the step (3), 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 (2) and the step (3), 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 (3) further includes that the nanocrystalline magnet core progress impregnation after step (4) will be heat-treated again is consolidated later
Change processing.
In the step (4), 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.
Embodiment 6
The present embodiment and above-described embodiment 1 the difference is that:
In the step (1), nanocrystalline strip is iron nickel base nanometer crystal zone material, and iron nickel base nanometer crystal zone material includes such as
The element of lower weight percent: Ni:15%, Si:10%, B:3%, Nb:2%, Cu:0.3%, Co:4%, surplus Fe.
Iron nickel base nanometer crystal zone material further 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%.
Embodiment 7
The present embodiment and above-described embodiment 2 the difference is that:
In the step (1), nanocrystalline strip is iron nickel base nanometer crystal zone material, and iron nickel base nanometer crystal zone material includes such as
The element of lower weight percent: Ni:18%, Si:11.5%, B:3.5%, Nb:2.5%, Cu:0.35%, Co:5%, surplus Fe.
Iron nickel base nanometer crystal zone material 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%.
Embodiment 8
The present embodiment and above-described embodiment 3 the difference is that:
In the step (1), nanocrystalline strip is iron nickel base nanometer crystal zone material, and iron nickel base nanometer crystal zone material includes such as
The element of lower weight percent: Ni:20%, Si:11%, B:4%, Nb:3%, Cu:0.4%, Co:6%, surplus Fe.
Iron nickel base nanometer crystal zone material further 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%.
Embodiment 9
The present embodiment and above-described embodiment 4 the difference is that:
In the step (1), nanocrystalline strip is iron nickel base nanometer crystal zone material, and iron nickel base nanometer crystal zone material includes such as
The element of lower weight percent: Ni:22%, Si:11.5%, B:4.5%, Nb:3.5%, Cu:0.45%, Co:7%, surplus Fe.
Iron nickel base nanometer crystal zone material 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%.
Embodiment 10
The present embodiment and above-described embodiment 5 the difference is that:
In the step (1), nanocrystalline strip is iron nickel base nanometer crystal zone material, and iron nickel base nanometer crystal zone material includes such as
The element of lower weight percent: Ni:25%, Si:12%, B:5%, Nb:4%, Cu:0.5%, Co:8%, surplus Fe.
Iron nickel base nanometer crystal zone material further 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%.
After tested, the Effective permeability μ e of nanocrystalline magnet core produced by the present invention can achieve 8.5 × 104More than, saturation
Magnetic induction value Bs can achieve 1.46T or more, and the value of coercivity magnetic field strength Hc is less than 2Am-1, remanence ratio is less than 0.07；It is anti-straight
Stream biasing ability is strong, and under 100Oe field strength, magnetic conductivity still has 72% or more；Wherein loss value under the conditions of 0.2T, 20k Hz
For 1.0W/kg hereinafter, magnetic core loss value under the conditions of 0.5T, 20k Hz is 5.2W/kg hereinafter, magnetic core is in 0.5T, 50k simultaneously
Loss value is 16.0W/kg or less under the conditions of Hz.
Nanocrystalline magnet core made from annealing process through the invention has stable magnetic conductivity and direct current biasing ability, also
Have many advantages, such as high saturated magnetic 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 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 (4)
1. a kind of annealing process for the remanent magnetism for reducing nanocrystalline magnet core, characterized by the following steps:
(1) nanocrystalline strip is wound into circular nano crystalline substance magnetic core；
(2) nanocrystalline magnet core is put into vacuum annealing furnace and is heat-treated；
(3) nanocrystalline magnet core after heat treatment is put into vacuum annealing furnace and is heat-treated again；
Wherein, in the step (1), nanocrystalline strip with a thickness of 15-25 μm, width 20-30mm；
Wherein, in the step (1), nanocrystalline strip is iron based nano crystal band, and the iron based nano crystal band includes as follows
The element of weight percent: Ni:15%-25%, Si:10%-12%, B:3%-5%, Nb:2%-4%, Cu:0.3%-
0.5%, Co:4%-8%, surplus Fe；
Wherein, in the step (2) and the step (3), 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 annealing process of remanent magnetism for reducing nanocrystalline magnet core according to claim 1, it is characterised in that: the step
Suddenly in (2) and the step (3), 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 nanocrystalline magnet core
It 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.
3. a kind of annealing process of remanent magnetism for reducing nanocrystalline magnet core according to claim 1, it is characterised in that: the step
Suddenly in (2) and the step (3), the vacuum degree in vacuum annealing furnace is less than -0.1Mpa, and vacuum annealing furnace is interior filled with gaseous mixture
Body, the nitrogen that the hydrogen and percent by volume that mixed gas is 10%-20% by percent by volume are 80%-90% form.
4. a kind of annealing process of remanent magnetism for reducing nanocrystalline magnet core according to claim 1, it is characterised in that: the step
It suddenly further include the nanocrystalline magnet core progress impregnation curing process after step (4) will be heat-treated again after (3).
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| CN106558415A (en) * | 2016-11-21 | 2017-04-05 | 东莞市大忠电子有限公司 | A kind of manufacture method of nanocrystalline common mode inductance |
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