CN102744403A - Preparation method of nanocrystalline magnetic powder cores - Google Patents
Preparation method of nanocrystalline magnetic powder cores Download PDFInfo
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- CN102744403A CN102744403A CN2012102037726A CN201210203772A CN102744403A CN 102744403 A CN102744403 A CN 102744403A CN 2012102037726 A CN2012102037726 A CN 2012102037726A CN 201210203772 A CN201210203772 A CN 201210203772A CN 102744403 A CN102744403 A CN 102744403A
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Abstract
The invention relates to a preparation method of nanocrystalline magnetic powder cores. According to the preparation method, non-crystalline strip materials with Fe<73.5>Cu1Nb3Si<13.5>B9 as ingredients are subjected to heat treatment in a vacuum heat treatment furnace and are cooled along with the furnace, crystallized nanocrystalline strips are subjected to ball milling in a planetary ball milling machine, nanocrystalline powder with different particle sizes are obtained through sieving, the nanocrystalline powder is passivated in phosphorizing liquid and is dried, the nanocrystalline powder with phosphate films is obtained, the nanocrystalline powder with phosphate films is uniformly mixed with insulation agents and bonding agents, the uniformly mixed powder is put in a mold to be pressed and formed, the formed magnetic powder is subjected to heat treatment under the protection of vacuum and inert gas, the magnetic powder subjected to the heat treatment is dipped in insulation glue, the outer layer of the magnetic powder subjected to the insulation curing is dipped with paint or is sprayed and coated with a layer of film, and the magnetic powder cores are obtained. Compared with the prior art, the preparation method has the advantage that the nanocrystalline magnetic powder cores prepared by the preparation method have high saturated magnetic induction intensity, low high-frequency loss and good stability.
Description
Technical field
The present invention relates to a kind of preparation method of nano magnetic material, especially relate to a kind of preparation method of nanocrystalline magnetic core.
Background technology
The magnetic core is a kind of by after the soft magnetic powder process insulation coating, through a kind of compound soft magnetic material of powder metallurgy process preparation.Because ferromagnetic particle is very little, is separated by non magnetic electrical insulating film material again.Therefore, can completely cut off eddy current on the one hand, material is applicable to upper frequency; On the other hand because the channel effect between the particle causes material to have lower magnetic conductivity and permanent permeance; Little owing to particle size again, the skin phenomenon that do not become basically, magnetic conductivity is also comparatively stable with change of frequency.It has, and high-frequency loss is little, temperature stability good, magnetic conductivity is little with change of frequency, saturation flux density is high, the constant zone of magnetic conductivity is wide, and magnetic conductivity can advantage such as regulate through the ratio of dielectric and ferromagnetic powder.Therefore, the magnetic core can be widely used in the production of various electronic devices and components such as communication, the energy, auto industry, household appliances, automatic gate and inductor, wave filter, transformer, inverter.
Amorphous nanocrystalline soft magnetic material is a kind of environment-friendly material that immediate development is got up, and is the substitute products that traditional soft magnetic materials comprises silicon steel, ferrite and permalloy etc., has all obtained remarkable breakthrough in theory research and application study field.The amorphous nano peritectic alloy has excellent soft magnet performance, with low cost, advantage such as technology is simple because of it, has made outstanding contribution for the conventional modified of China and new and high technology develop cause rapidly.Along with the development towards miniaturization, lightweight direction of electronic equipment, electronic instrument, nano-crystal soft magnetic alloy highlights its increasing advantage with its high magnetic permeability, low high-frequency loss with than performance characteristics such as high saturated magnetic inductions.Nano-crystal soft magnetic alloy magnetic core has obtained successful Application in the powerful field of the big electric current of high frequency, like boost ring and the filter inductance of ups power, filter inductance and energy storage inductor, the oil field high power switching power supply filter inductance etc. of military Switching Power Supply.
In recent years, the exploitation of amorphous, nanocrystalline magnetic core all is devoted in a lot of researchs, and major side overweights the magnetic core and prepares powder size in the process, binding agent kind and content, briquetting pressure, Technology for Heating Processing etc.Few about the powder passivation to the influence research of magnetic core.Generated the very thin phosphating coat of one deck after the powder passivation,, can make the excellence conductor of metal surface change non-conductor into because it is the nonmetallic non-conductive separation layer of one deck; Increased the resistivity of nano-crystalline granule; Help the magnetic core loss and reduce, frequency characteristic is stable, and quality factor increase.
Summary of the invention
The object of the invention is exactly that a kind of preparation method with nanocrystalline magnetic core of high saturation induction density, low high-frequency loss, good stable property is provided in order to overcome the defective that above-mentioned prior art exists.
The object of the invention can be realized through following technical scheme:
A kind of preparation method of nanocrystalline magnetic core may further comprise the steps:
(1) crystallization is handled: with composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band heat treatment and with stove cooling in vacuum heat treatment furnace, obtain the nanometer crystal zone after the crystallization;
(2) ball-milling treatment: with the ball milling in the star formula ball mill of being expert at of the nanometer crystal zone after the crystallization, screening obtains varigrained manocrystalline powders;
(3) passivation: with manocrystalline powders passivation 0.5～1 hour in phosphatization liquid, and oven dry, obtain having the manocrystalline powders of phosphating coat;
(4) mix: the manocrystalline powders that will have phosphating coat mixes the powder that obtains mixing with insulating compound and binding agent;
(5) moulding: the powder that mixes is put into mould compression moulding, obtain the magnetic core of compression moulding;
(6) heat treatment: the magnetic core of compression moulding is heat-treated under vacuum or inert gas shielding, obtain the magnetic core after the heat treatment;
(7) insulation is solidified: the magnetic core after the heat treatment was flooded in insulating cement 1～3 hour, and magnetic core after solidifying obtains insulating;
(8) packing: outer dipping lacquer of the magnetic core after insulation is solidified or spraying thin film obtain nanocrystalline magnetic core.
The required temperature of the described heat treatment of step (1) is 500～600 ℃, and the required time of heat treatment is 0.5 hour.
The process conditions of the described ball-milling treatment of step (2) are: material ball ratio 1: 50, the deep bid rotating speed of planetary ball mill is 180 rev/mins, 3 hours ball milling time.
The phosphoric acid solution that the described phosphatization liquid of step (3) is 3wt%.
The described mass ratio that has manocrystalline powders, insulating compound and the binding agent of phosphating coat of step (4) is 1: 1%～5%: 1%～10%.
The described insulating compound of step (4) is the mixture of mica and zinc stearate, and binding agent is a polyimide resin.
In the forming process of step (5), slowly exert pressure, reached after the briquetting pressure pressurize 3～5 minutes, briquetting pressure is 500～1000Mpa.
The required temperature of the described heat treatment of step (6) is 100～550 ℃, and the required time of heat treatment is 0.5～3 hour.
The described inert gas of step (6) is an argon gas.
The described insulating cement of step (7) is an epoxy resin.
Detect the magnetic property of the magnetic core after packing, comprise initial permeability, quality factor etc.Adopt crushing strength that the intensity of magnetic core is tested.
Compared with prior art, the present invention adopts phosphoric acid solution passivation powder, makes the manocrystalline powders surface generate the very thin phosphate coating of one deck, has improved the resistivity between the powder particle, helps reducing the high-frequency vortex loss of magnetic core, increases quality factor; The magnetic core of the present invention preparation has improved nanocrystalline magnetic core and has been difficult for shortcomings such as compression moulding, packing are low, formability difference, and the nanocrystalline magnetic core of the present invention's preparation has high saturation induction density, low high-frequency loss, good stable property.
Description of drawings
Fig. 1 generates ferric phosphate film transmission electron microscope figure after the manocrystalline powders of embodiment 1 advances transpassivation.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Embodiment 1
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.Ferromagnetic powder surface after the passivation forms the phosphating coat about one deck 100nm, and the manocrystalline powders transmission electron microscope photo that generates phosphating coat is as shown in Figure 1, and light gray areas is phosphating coat among the figure.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 400 ℃.Magnetic core after the heat treatment flooded in epoxy resin 1 hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 2:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 10% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 400 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 3:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 15% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 400 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 4:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 700MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 400 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 5:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 500MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 400 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 6:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 300 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 7:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 350 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 8:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 400 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 9:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 450 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 10:
With composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band in vacuum heat treatment furnace, heat-treat, heat treatment temperature is 550 ℃ * 0.5 hour, cools off with stove.Nanometer crystal zone after the crystallization is expert at carries out ball milling in the star formula ball mill.Material ball ratio 1: 50,180 rev/mins of deep bid rotating speeds, 3 hours ball milling time, the manocrystalline powders that adopts ball milling to make adds mass fraction and is in 3% the phosphoric acid solution, stirs 0.5h, oven dry.The organic siliconresin of the powder after the oven dry and 0.5% mica, 5% modification, 0.5% zinc stearate are mixed, and abundant stirring coats powder surface fully.The powder that obtains is pressed into the annular of φ 20.3 * 12.7 * 6.35mm in mould, briquetting pressure 1000MPa, the magnetic core of moulding is taken out in pressurize after 3 minutes.Under argon shield, heat-treat temperature retention time 1 hour for 500 ℃.Magnetic core after the heat treatment flooded in epoxy resin one hour, after insulation is solidified, at the thick epoxy resin of magnetic core outer brush one deck 1mm, wait solidify fully after, the magnetic core is packed.The performance parameter of specimen.
Embodiment 11
A kind of preparation method of nanocrystalline magnetic core may further comprise the steps: (1) crystallization is handled: with composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band heat treatment and with stove cooling in vacuum heat treatment furnace, obtain the nanometer crystal zone after the crystallization; (2) ball-milling treatment: with the ball milling in the star formula ball mill of being expert at of the nanometer crystal zone after the crystallization, screening obtains varigrained manocrystalline powders; (3) passivation: with manocrystalline powders passivation 0.5 hour in phosphatization liquid, and oven dry, obtain having the manocrystalline powders of phosphating coat; (4) mix: the manocrystalline powders that will have phosphating coat mixes the powder that obtains mixing with insulating compound and binding agent; (5) moulding: the powder that mixes is put into mould compression moulding, obtain the magnetic core of compression moulding; (6) heat treatment: the magnetic core of compression moulding is heat-treated under vacuum or inert gas shielding, obtain the magnetic core after the heat treatment; (7) insulation is solidified: the magnetic core after the heat treatment flood 1 hour the magnetic core after the curing that obtains insulating in insulating cement; (8) packing: outer dipping lacquer of the magnetic core after insulation is solidified or spraying thin film obtain nanocrystalline magnetic core.
The required temperature of the described heat treatment of step (1) is 500 ℃, and the required time of heat treatment is 0.5 hour.The process conditions of the described ball-milling treatment of step (2) are: material ball ratio 1: 50, the deep bid rotating speed of planetary ball mill is 180 rev/mins, 3 hours ball milling time.The phosphoric acid solution that the described phosphatization liquid of step (3) is 3wt%.The described mass ratio that has manocrystalline powders, insulating compound and the binding agent of phosphating coat of step (4) is 1: 1%: 1%.The described insulating compound of step (4) is the mixture of mica and zinc stearate, and binding agent is a polyimide resin.In the forming process of step (5), slowly exert pressure, reached after the briquetting pressure pressurize 5 minutes, briquetting pressure is 500Mpa.The required temperature of the described heat treatment of step (6) is 100 ℃, and the required time of heat treatment is 3 hours.The described inert gas of step (6) is an argon gas.The described insulating cement of step (7) is an epoxy resin.Detect the magnetic property of the magnetic core after packing, comprise initial permeability, quality factor etc.Adopt crushing strength that the intensity of magnetic core is tested.
Embodiment 12
A kind of preparation method of nanocrystalline magnetic core may further comprise the steps: (1) crystallization is handled: with composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band heat treatment and with stove cooling in vacuum heat treatment furnace, obtain the nanometer crystal zone after the crystallization; (2) ball-milling treatment: with the ball milling in the star formula ball mill of being expert at of the nanometer crystal zone after the crystallization, screening obtains varigrained manocrystalline powders; (3) passivation: with manocrystalline powders passivation 1 hour in phosphatization liquid, and oven dry, obtain having the manocrystalline powders of phosphating coat; (4) mix: the manocrystalline powders that will have phosphating coat mixes the powder that obtains mixing with insulating compound and binding agent; (5) moulding: the powder that mixes is put into mould compression moulding, obtain the magnetic core of compression moulding; (6) heat treatment: the magnetic core of compression moulding is heat-treated under vacuum or inert gas shielding, obtain the magnetic core after the heat treatment; (7) insulation is solidified: the magnetic core after the heat treatment flood 2 hours the magnetic core after the curing that obtains insulating in insulating cement; (8) packing: outer dipping lacquer of the magnetic core after insulation is solidified or spraying thin film obtain nanocrystalline magnetic core.
The required temperature of the described heat treatment of step (1) is 550 ℃, and the required time of heat treatment is 0.5 hour.The process conditions of the described ball-milling treatment of step (2) are: material ball ratio 1: 50, the deep bid rotating speed of planetary ball mill is 180 rev/mins, 3 hours ball milling time.The phosphoric acid solution that the described phosphatization liquid of step (3) is 3wt%.The described mass ratio that has manocrystalline powders, insulating compound and the binding agent of phosphating coat of step (4) is 1: 3%: 5%.Step (3) phosphating coat thickness is 100nm.The described insulating compound of step (4) is the mixture of mica and zinc stearate, and binding agent is a polyimide resin.In the forming process of step (5), slowly exert pressure, reached after the briquetting pressure pressurize 4 minutes, briquetting pressure is 800Mpa.The required temperature of the described heat treatment of step (6) is 350 ℃, and the required time of heat treatment is 2 hours.The described inert gas of step (6) is an argon gas.The described insulating cement of step (7) is an epoxy resin.Detect the magnetic property of the magnetic core after packing.
Embodiment 13
A kind of preparation method of nanocrystalline magnetic core may further comprise the steps: (1) crystallization is handled: with composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band heat treatment and with stove cooling in vacuum heat treatment furnace, obtain the nanometer crystal zone after the crystallization; (2) ball-milling treatment: with the ball milling in the star formula ball mill of being expert at of the nanometer crystal zone after the crystallization, screening obtains varigrained manocrystalline powders; (3) passivation: with manocrystalline powders passivation 1 hour in phosphatization liquid, and oven dry, obtain having the manocrystalline powders of phosphating coat; (4) mix: the manocrystalline powders that will have phosphating coat mixes the powder that obtains mixing with insulating compound and binding agent; (5) moulding: the powder that mixes is put into mould compression moulding, obtain the magnetic core of compression moulding; (6) heat treatment: the magnetic core of compression moulding is heat-treated under vacuum or inert gas shielding, obtain the magnetic core after the heat treatment; (7) insulation is solidified: the magnetic core after the heat treatment flood 3 hours the magnetic core after the curing that obtains insulating in insulating cement; (8) packing: outer dipping lacquer of the magnetic core after insulation is solidified or spraying thin film obtain nanocrystalline magnetic core.
The required temperature of the described heat treatment of step (1) is 600 ℃, and the required time of heat treatment is 0.5 hour.The process conditions of the described ball-milling treatment of step (2) are: material ball ratio 1: 50, the deep bid rotating speed of planetary ball mill is 180 rev/mins, 3 hours ball milling time.The phosphoric acid solution that the described phosphatization liquid of step (3) is 3wt%.Step (3) phosphating coat thickness is 120nm.The described mass ratio that has manocrystalline powders, insulating compound and the binding agent of phosphating coat of step (4) is 1: 5%: 10%.The described insulating compound of step (4) is the mixture of mica and zinc stearate, and binding agent is a polyimide resin.In the forming process of step (5), slowly exert pressure, reached after the briquetting pressure pressurize 3 minutes, briquetting pressure is 1000Mpa.The required temperature of the described heat treatment of step (6) is 550 ℃, and the required time of heat treatment is 0.5 hour.The described inert gas of step (6) is an argon gas.The described insulating cement of step (7) is an epoxy resin.Adopt crushing strength that the intensity of magnetic core is tested.
Claims (10)
1. the preparation method of a nanocrystalline magnetic core is characterized in that, this method may further comprise the steps:
(1) crystallization is handled: with composition is Fe
73.5Cu
1Nb
3Si
13.5B
9Amorphous band heat treatment and with stove cooling in vacuum heat treatment furnace, obtain the nanometer crystal zone after the crystallization;
(2) ball-milling treatment: with the ball milling in the star formula ball mill of being expert at of the nanometer crystal zone after the crystallization, screening obtains varigrained manocrystalline powders;
(3) passivation: with manocrystalline powders passivation 0.5～1 hour in phosphatization liquid, and oven dry, obtain having the manocrystalline powders of phosphating coat;
(4) mix: the manocrystalline powders that will have phosphating coat mixes the powder that obtains mixing with insulating compound and binding agent;
(5) moulding: the powder that mixes is put into mould compression moulding, obtain the magnetic core of compression moulding;
(6) heat treatment: the magnetic core of compression moulding is heat-treated under vacuum or inert gas shielding, obtain the magnetic core after the heat treatment;
(7) insulation is solidified: the magnetic core after the heat treatment was flooded in insulating cement 1～3 hour, and magnetic core after solidifying obtains insulating;
(8) packing: outer dipping lacquer of the magnetic core after insulation is solidified or spraying thin film obtain nanocrystalline magnetic core.
2. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the required temperature of the described heat treatment of step (1) is 500～600 ℃, and the required time of heat treatment is 0.5 hour.
3. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the process conditions of the described ball-milling treatment of step (2) are: material ball ratio 1: 50, the deep bid rotating speed of planetary ball mill is 180 rev/mins, 3 hours ball milling time.
4. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the phosphoric acid solution that the described phosphatization liquid of step (3) is 3wt%.
5. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the described mass ratio that has manocrystalline powders, insulating compound and the binding agent of phosphating coat of step (4) is 1: 1%～5%: 1%～10%.
6. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the described insulating compound of step (4) is the mixture of mica and zinc stearate, and binding agent is a polyimide resin.
7. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, in the forming process of step (5), slowly exerts pressure, and reaches after the briquetting pressure pressurize 3～5 minutes, and briquetting pressure is 500～1000Mpa.
8. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the required temperature of the described heat treatment of step (6) is 100～550 ℃, and the required time of heat treatment is 0.5～3 hour.
9. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the described inert gas of step (6) is an argon gas.
10. the preparation method of a kind of nanocrystalline magnetic core according to claim 1 is characterized in that, the described insulating cement of step (7) is an epoxy resin.
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| CN103065789A (en) * | 2012-12-21 | 2013-04-24 | 内蒙古工业大学 | Preparation and coating method of high-performance iron-based amorphous metal powder core |
| CN103456480A (en) * | 2013-08-28 | 2013-12-18 | 黑龙江八一农垦大学 | One-step heat treatment preparation process method for soft nanocrystalline magnetic powder core |
| CN103567436A (en) * | 2013-11-28 | 2014-02-12 | 四川东阁科技有限公司 | Manufacturing method of iron-silicon material and iron-silicon magnetic powder core having permeability mu of 55 |
| CN103692705A (en) * | 2013-12-16 | 2014-04-02 | 杨全民 | Composite magnetic material and preparation method and use thereof |
| CN103745791A (en) * | 2013-12-27 | 2014-04-23 | 青岛云路新能源科技有限公司 | Production method of ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core |
| CN104368807A (en) * | 2013-08-13 | 2015-02-25 | 东睦新材料集团股份有限公司 | Power coating method of metal soft magnetic composite and preparing method of metal soft magnetic composite |
| CN104513479A (en) * | 2014-12-19 | 2015-04-15 | 广东奇德新材料股份有限公司 | Preparation method of PA6 nano-composite material with magnetic property |
| CN104513477A (en) * | 2014-12-19 | 2015-04-15 | 广东奇德新材料股份有限公司 | PA6 nano-composite material with magnetic property |
| CN106816252A (en) * | 2016-12-29 | 2017-06-09 | 天通控股股份有限公司 | A kind of manufacture method of insulaion resistance FeSiCr metal soft magnetic materials high |
| CN107936558A (en) * | 2017-12-13 | 2018-04-20 | 江西伟普科技有限公司 | A kind of preparation method of the high temperature resistant injection molding adhesion magnetic material of high magnetic applications scope |
| DE112018001808T5 (en) | 2017-11-29 | 2019-12-19 | Grirem Advanced Materials Co., Ltd. | Rare earth-bonded magnetic powder and manufacturing process therefor and bonded magnet |
| CN111009371A (en) * | 2019-12-27 | 2020-04-14 | 浙江工业大学 | Preparation method of soft magnetic composite material based on novel phosphating solution process |
| CN112908603A (en) * | 2021-01-21 | 2021-06-04 | 广东省科学院材料与加工研究所 | Iron-based amorphous magnetic powder core and preparation method thereof |
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| CN103065789A (en) * | 2012-12-21 | 2013-04-24 | 内蒙古工业大学 | Preparation and coating method of high-performance iron-based amorphous metal powder core |
| CN103065789B (en) * | 2012-12-21 | 2016-08-03 | 内蒙古工业大学 | The preparation of a kind of high-performance iron based non-crystalline metal powder core and coating process |
| CN104368807A (en) * | 2013-08-13 | 2015-02-25 | 东睦新材料集团股份有限公司 | Power coating method of metal soft magnetic composite and preparing method of metal soft magnetic composite |
| CN103456480A (en) * | 2013-08-28 | 2013-12-18 | 黑龙江八一农垦大学 | One-step heat treatment preparation process method for soft nanocrystalline magnetic powder core |
| CN103567436A (en) * | 2013-11-28 | 2014-02-12 | 四川东阁科技有限公司 | Manufacturing method of iron-silicon material and iron-silicon magnetic powder core having permeability mu of 55 |
| CN103692705B (en) * | 2013-12-16 | 2015-06-03 | 杨全民 | Composite magnetic material and preparation method and use thereof |
| CN103692705A (en) * | 2013-12-16 | 2014-04-02 | 杨全民 | Composite magnetic material and preparation method and use thereof |
| CN103745791A (en) * | 2013-12-27 | 2014-04-23 | 青岛云路新能源科技有限公司 | Production method of ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core |
| CN104513477A (en) * | 2014-12-19 | 2015-04-15 | 广东奇德新材料股份有限公司 | PA6 nano-composite material with magnetic property |
| CN104513479A (en) * | 2014-12-19 | 2015-04-15 | 广东奇德新材料股份有限公司 | Preparation method of PA6 nano-composite material with magnetic property |
| CN106816252A (en) * | 2016-12-29 | 2017-06-09 | 天通控股股份有限公司 | A kind of manufacture method of insulaion resistance FeSiCr metal soft magnetic materials high |
| CN106816252B (en) * | 2016-12-29 | 2018-10-09 | 天通控股股份有限公司 | A kind of manufacturing method of high insulation resistance FeSiCr metal soft magnetic materials |
| DE112018001808T5 (en) | 2017-11-29 | 2019-12-19 | Grirem Advanced Materials Co., Ltd. | Rare earth-bonded magnetic powder and manufacturing process therefor and bonded magnet |
| CN107936558A (en) * | 2017-12-13 | 2018-04-20 | 江西伟普科技有限公司 | A kind of preparation method of the high temperature resistant injection molding adhesion magnetic material of high magnetic applications scope |
| CN111009371A (en) * | 2019-12-27 | 2020-04-14 | 浙江工业大学 | Preparation method of soft magnetic composite material based on novel phosphating solution process |
| CN112908603A (en) * | 2021-01-21 | 2021-06-04 | 广东省科学院材料与加工研究所 | Iron-based amorphous magnetic powder core and preparation method thereof |
| CN112908603B (en) * | 2021-01-21 | 2023-09-26 | 广东省科学院材料与加工研究所 | Iron-based amorphous magnetic powder core and preparation method thereof |
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