CN105810383A - Preparation method for iron-based nanocrystalline magnetic powder core - Google Patents
Preparation method for iron-based nanocrystalline magnetic powder core Download PDFInfo
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Abstract
The invention discloses a preparation method for an iron-based nanocrystalline magnetic powder core. The preparation method comprises the following steps of preparing iron-based amorphous alloy powder by FeSiBPNbCu alloy with high amorphous forming capacity through a gas atomization method; screening and matching the iron-based amorphous alloy; carrying out passivation and insulation coating processing on the powder through a passivant, an insulating compound and a binder; and then pressing and forming, and carrying out crystallization processing on the powder. According to the preparation method, the iron-based amorphous alloy powder is prepared by the gas atomization method; the prepared powder has the characteristics of high degree of sphericity and low oxygen content; the powder can be insulated and coated easily, so that the problem of sharp corners and difficulty in insulation of the powder adopted by the conventional nanocrystalline magnetic powder core when the powder is processed by a strip crushing method is solved; therefore, the loss of the magnetic powder core is lowered consequently; and in addition, the iron-based nanocrystalline magnetic powder core is stable in magnetic conductivity, low in iron core loss, excellent in direct current bias resistance, excellent in comprehensive performance, and is expected to be used as various inductance elements with functions of filtering, current stabilizing, energy storing and the like for various switch power supply modules.
Description
Technical field
The present invention relates to field of magnetic material, the preparation method particularly relating to a kind of iron based nano crystal powder core.
Background technology
Iron-based amorphous and nanocrystalline soft magnetic alloy has the advantages such as saturation induction density height, initial permeability is high, coercivity is little, loss is low, the iron core that the amorphous band prepared with quick quenching technique turns to has excellent soft magnet performance after suitable heat treatment, is widely used in fields such as all kinds of transformators, sensor, Switching Power Supplies.But along with electron electric power industrial expansion, electronic device is to miniaturization, high frequency and big sense of current development, and band is very big around soft magnet core loss when high-frequency work of, lamination, limits its application in high frequency.At this time, it may be necessary to adopt powder core to meet work requirements.Powder core is to adopt powder metallurgical technique, soft-magnetic alloy powder and dielectric mix compacting.Traditional powder core mainly has ferrocart core, ferrum silica flour core, ferrum Si-Al Magnetic Powder Core, ferrum nikel powder core and FeNiCo magnetic core etc..Ferrocart core is cheap, but high frequency characteristics and loss characteristic are not good;Ferrum silica flour core is moderate, DC stacked excellent performance, but high-frequency loss is high;Ferrum Si-Al Magnetic Powder Core wide application, loss is low, and frequency performance is good, has excellent cost performance, but DC superposition characteristic is not ideal enough;Ferrum nikel powder core has the D.C. magnetic biasing characteristic of the best, but price is higher, and loss is also high;Ferrum nickel molybdenum best performance is got over, but price is also the most expensive, and fancy price limits its range of application.
Iron-based amorphous nanometer crystalline powder core is the Novel magnetic powder core that latest developments are got up, and has the features such as high intensity, high rigidity and good soft magnet performance, and with low cost, is increasingly becoming research and the focus of application in recent years.Application number is the patent of invention preparation method that discloses a kind of magnetically soft alloy powder core of 201310018768.7, processing including amorphous band embrittlement, be ground into the steps such as powder, screening and proportioning, Passivation Treatment and insulating wrapped, compressing, annealing and spraying, the high frequency performance of powder core is excellent.Application number is the patent of invention preparation method that discloses a kind of iron based nano crystal powder core with superhigh magnetic conductivity of 201310733299.7, by the method adopting the mixing of coarse powder, fine powder and coupling processing, effectively solve the problem that bulky grain manocrystalline powders is compressing, prepare pcrmeability of knowing clearly and reach the iron based nano crystal powder core with superhigh magnetic conductivity of more than 200, but the performance such as its core loss not announcing powder core and anti-direct current biasing ability.Application number be 201310280793.2 patent of invention disclose a kind of low-loss Fe base nanometer crystal powder core and preparation method thereof, it is prone to molding, it is beneficial to environmental protection, there is certain cost advantage, but the anti-direct current biasing ability of its nanocrystalline magnetic core is poor, when externally-applied magnetic field is 40Oe, its pcrmeability has decayed to less than 80% when not adding magnetic field.
The magnetic powder that the amorphous related in above-mentioned patent and nanocrystalline magnetic core adopt all is prepared by band crush method, the process of ball mill crushing is readily incorporated impurity, cause that the component of powder is uneven, colleague, the powder obtained mostly is the lamellar with corner angle, being difficult to insulate, cause that the loss of powder core is higher, anti-direct current biasing ability is poor.
Summary of the invention
For solving the problems referred to above, the preparation method that it is an object of the invention to provide a kind of iron based nano crystal powder core, it is characterised in that comprise the steps:
(1) to the Composition of Fe-Based Amorphous Alloy with large-amorphous forming capacity, aerosolization method is adopted to prepare Fe-based amorphous alloy powder；
(2) the Fe-based amorphous alloy powder of target grain size is obtained by screening after the Fe-based amorphous alloy powder of preparation being processed；
(3) adopt passivator to be passivated processing to the Fe-based amorphous alloy powder after screening, then use insulating compound and binding agent that the Fe-based amorphous alloy powder after Passivation Treatment is carried out insulating wrapped process；
(4) by after the Fe-based amorphous alloy powder pressing forming handled well, annealing is carried out, it is thus achieved that iron based nano crystal powder core.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, the mass percent of each element in the Composition of Fe-Based Amorphous Alloy of large-amorphous forming capacity that has in described step (1) is 4.5 ~ 5.5%Si, 2 ~ 4%B, 2.5 ~ 4%P, 1.5 ~ 2.5%Nb, 0.5 ~ 1%Cu, surplus is Fe.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, in described step (1), before adopting aerosolization method to prepare Fe-based amorphous alloy powder, the Composition of Fe-Based Amorphous Alloy with large-amorphous forming capacity is heated to more than fusing point 150 ~ 300 DEG C, and is incubated 10 ~ 30min.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, it is 5 ~ 15MPa that the aerosolization method in described step (1) prepares the atomizing pressure of Fe-based amorphous alloy powder, and melt nozzle diameter is 0.5 ~ 3mm.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, in described step (2), the Fe-based amorphous alloy powder of target grain size is the powder by 200 eye mesh screens, and namely powder diameter is less than 75 μm.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, in described step (3), passivator is Phosphating Solution, and described insulating compound is mica powder, and described binding agent is epoxy resin or polyamide.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, pressure compressing in described step (4) is 10 ~ 26t/cm2, and the dwell time is 5 ~ 30s.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, in described step (4), the temperature of annealing is 460 ~ 530 DEG C, and the process time is 0.5 ~ 3 hour.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, in described step (4), the atmosphere of subsequent annealing can be the reducing atmospheres such as the protective atmosphere such as nitrogen, argon or hydrogen.
Further, the preparation method of iron based nano crystal powder core according to above-mentioned design, in described step (3), processing procedure to Fe-based amorphous alloy powder is joined by Fe-based amorphous alloy powder in the Phosphating Solution of 1 ~ 10%, it is evenly stirred until dry, subsequently by the Muscovitum Homogeneous phase mixing of the Fe-based amorphous alloy powder after Passivation Treatment and 1 ~ 5%, obtain mixed-powder, finally, mixed-powder is joined in the epoxy resin of 1 ~ 5% or the acetone soln of polyamide, be evenly stirred until dry.
Preparation method provided by the invention has the advantages that 1, the amorphous formation ability of alloy is high, aerosolization method is adopted to prepare Fe-based amorphous alloy powder, can avoid what conventional tape crush method existed to be mixed into impurity, uneven components and the problem that there is sharp corners, it is beneficial to the insulating wrapped of powder, thus reducing the core loss of powder core, improve its anti-direct current biasing ability.2, by compressing and annealing, the iron based nano crystal powder core that even tissue, high intensity, high-compactness and pcrmeability are constant is obtained, the various inductance elements such as filtering, current stabilization and energy storage being expected to be used as on various switch power module.
Accompanying drawing explanation
Fig. 1 is the SEM exterior appearance figure of the Fe-based amorphous alloy powder of preparation in embodiment 1.
Fig. 2 is the XRD figure spectrum of the Fe-based amorphous alloy powder of preparation in embodiment 1.
Fig. 3 is the pcrmeability variation tendency with externally-applied magnetic field of embodiment 1 iron based nano crystal powder core.
Detailed description of the invention
Below according to the preferred embodiment of the present invention, the preparation method of iron based nano crystal powder core is illustrated.
Embodiment 1:
Foundry alloy heating being melted to more than fusing point 200 DEG C and be incubated 10 minutes, adopting aerosolization method to prepare FeSiBPNbCu alloy powder, the pressure of aerosolization is 10MPa, nozzle diameter is 1mm, by alloy powder in vacuum drying oven dried, with 200 eye mesh screens, powder is sieved, it is thus achieved that target powder, by scanning electron microscope (SEM), the pattern of target powder is analyzed, as shown in Figure 1, it can be seen that powder presents spherical, smooth surface, without defects such as obvious hole, holes；Detecting its structure with X-ray diffractometer (XRD), result, as shown in fig. 2, it can be seen that XRD figure composes the diffraction maximum not having any crystalline phase corresponding, only has a wide diffusing scattering peak, illustrates that prepared powder is completely amorphous state.
Amorphous powder being passivated and insulating wrapped processes, Passivation Treatment: poured into by amorphous powder in the Phosphating Solution of 1wt%, at the uniform velocity stirring is until drying；Insulating wrapped: joined by the amorphous powder after Passivation Treatment in the polyamide acetone soln of 1wt% epoxy resin and 1wt%, at the uniform velocity stirring is to dry.After insulating wrapped, through the screen cloth rescreening of 100 orders, the powder particle collecting below 100 orders is pressed.
Powder particle is put in hydraulic forming machine, use 18t/cm2Pressure be pressed into external diameter 20.3mm, internal diameter 12.7mm, be highly 6.35mm(Φ 20.3 × 12.7 × 6.35mm) annular powder core, the dwell time is 10s, and after molding, the surface composition of powder core is uniform, no significant defect.After the powder core of described molding carries out the annealing of 1 hour at 510 DEG C, it is thus achieved that iron based nano crystal powder core, detecting through XRD, Crystallization Phases is single α-Fe phase.Measure the performances such as the pcrmeability of powder core, loss and direct current biasing respectively.
After tested, powder core pcrmeability under 1MHz frequency is 72, and meanwhile, frequency stability is excellent；The loss of powder core is very low, and when 50kHz, 0.1T, loss is 740mW/cm3；Under 100Oe externally-applied magnetic field, pcrmeability remains to be maintained at 60% when not adding magnetic field, as shown in Figure 3, it is seen that, prepared new iron-based nanocrystalline magnetic core excellent combination property.
Embodiment 2:
Foundry alloy heating is melted to more than fusing point 150 DEG C and is incubated 15 minutes, aerosolization method is adopted to prepare FeSiBPNbCu alloy powder, the pressure of aerosolization is 12MPa, nozzle diameter is 1mm, by alloy powder in vacuum drying oven dried, with 200 eye mesh screens, powder is sieved, obtain target powder, SEM collection of illustrative plates display powder presents spherical, and smooth surface, without defects such as obvious hole, holes；Powder prepared by XRD figure spectrum display is completely amorphous state.
Amorphous powder being passivated and insulating wrapped processes, Passivation Treatment: poured into by amorphous powder in the Phosphating Solution of 1wt%, at the uniform velocity stirring is until drying；Insulating wrapped: joined by the amorphous powder after Passivation Treatment in the polyamide acetone soln of 1wt% epoxy resin and 1wt%, at the uniform velocity stirring is to dry.After insulating wrapped, through the screen cloth rescreening of 100 orders, the powder particle collecting below 100 orders is pressed.
Powder particle is put in hydraulic forming machine, use 18t/cm2Pressure be pressed into external diameter 20.3mm, internal diameter 12.7mm, be highly 6.35mm(Φ 20.3 × 12.7 × 6.35mm) annular powder core, the dwell time is 10s, and after molding, the surface composition of powder core is uniform, no significant defect.After the powder core of described molding carries out the annealing of 1 hour at 500 DEG C, it is thus achieved that iron based nano crystal powder core, detecting through XRD, Crystallization Phases is single α-Fe phase.Measure the performances such as the pcrmeability of powder core, loss and direct current biasing respectively.
After tested, powder core pcrmeability under 1MHz frequency is 65, and meanwhile, frequency stability is excellent；The loss of powder core is very low, and when 50kHz, 0.1T, loss is 700mW/cm3；Under 100Oe externally-applied magnetic field, pcrmeability remains to be maintained at 63% when not adding magnetic field.Visible, prepared new iron-based nanocrystalline magnetic core excellent combination property.
Embodiment 3:
Foundry alloy heating is melted to more than fusing point 200 DEG C and is incubated 8 minutes, aerosolization method is adopted to prepare FeSiBPNbCu alloy powder, the pressure of aerosolization is 9MPa, nozzle diameter is 1mm, by alloy powder in vacuum drying oven dried, with 200 eye mesh screens, powder is sieved, obtain target powder, SEM collection of illustrative plates display powder presents spherical, and smooth surface, without defects such as obvious hole, holes；Powder prepared by XRD figure spectrum display is completely amorphous state.
Amorphous powder being passivated and insulating wrapped processes, Passivation Treatment: poured into by amorphous powder in the Phosphating Solution of 1wt%, at the uniform velocity stirring is until drying；Insulating wrapped: joined by the amorphous powder after Passivation Treatment in the polyamide acetone soln of 1wt% epoxy resin and 1wt%, at the uniform velocity stirring is to dry.After insulating wrapped, through the screen cloth rescreening of 100 orders, the powder particle collecting below 100 orders is pressed.
Powder particle is put in hydraulic forming machine, use 20t/cm2Pressure be pressed into external diameter 20.3mm, internal diameter 12.7mm, be highly 6.35mm(Φ 20.3 × 12.7 × 6.35mm) annular powder core, the dwell time is 15s, and after molding, the surface composition of powder core is uniform, no significant defect.After the powder core of described molding carries out the annealing of 1 hour at 510 DEG C, it is thus achieved that iron based nano crystal powder core, detecting through XRD, Crystallization Phases is single α-Fe phase.Measure the performances such as the pcrmeability of powder core, loss and direct current biasing respectively.
After tested, powder core pcrmeability under 1MHz frequency is 75, and meanwhile, frequency stability is excellent；The loss of powder core is very low, and when 50kHz, 0.1T, loss is 720mW/cm3；Under 100Oe externally-applied magnetic field, pcrmeability remains to be maintained at 61% when not adding magnetic field.Visible, prepared new iron-based nanocrystalline magnetic core excellent combination property.
Embodiment 4:
Foundry alloy heating is melted to more than fusing point 250 DEG C and is incubated 5 minutes, aerosolization method is adopted to prepare FeSiBPNbCu alloy powder, the pressure of aerosolization is 11MPa, nozzle diameter is 1mm, by alloy powder in vacuum drying oven dried, with 200 eye mesh screens, powder is sieved, obtain target powder, SEM collection of illustrative plates display powder presents spherical, and smooth surface, without defects such as obvious hole, holes；Powder prepared by XRD figure spectrum display is completely amorphous state.
Amorphous powder being passivated and insulating wrapped processes, Passivation Treatment: poured into by amorphous powder in the Phosphating Solution of 1wt%, at the uniform velocity stirring is until drying；Insulating wrapped: joined by the amorphous powder after Passivation Treatment in the polyamide acetone soln of 1wt% epoxy resin and 1wt%, at the uniform velocity stirring is to dry.After insulating wrapped, through the screen cloth rescreening of 100 orders, the powder particle collecting below 100 orders is pressed.
Powder particle is put in hydraulic forming machine, use 17t/cm2Pressure be pressed into external diameter 20.3mm, internal diameter 12.7mm, be highly 6.35mm(Φ 20.3 × 12.7 × 6.35mm) annular powder core, the dwell time is 10s, and after molding, the surface composition of powder core is uniform, no significant defect.After the powder core of described molding carries out the annealing of 1 hour at 510 DEG C, it is thus achieved that iron based nano crystal powder core, detecting through XRD, Crystallization Phases is single α-Fe phase.Measure the performances such as the pcrmeability of powder core, loss and direct current biasing respectively.
After tested, powder core pcrmeability under 1MHz frequency is 68, and meanwhile, frequency stability is excellent；The loss of powder core is very low, and when 50kHz, 0.1T, loss is 760mW/cm3；Under 100Oe externally-applied magnetic field, pcrmeability remains to be maintained at 64% when not adding magnetic field.Visible, prepared new iron-based nanocrystalline magnetic core excellent combination property.
Embodiment 5:
Foundry alloy heating is melted to more than fusing point 200 DEG C and is incubated 15 minutes, aerosolization method is adopted to prepare FeSiBPNbCu alloy powder, the pressure of aerosolization is 10MPa, nozzle diameter is 1mm, by alloy powder in vacuum drying oven dried, with 200 eye mesh screens, powder is sieved, obtain target powder, SEM collection of illustrative plates display powder presents spherical, and smooth surface, without defects such as obvious hole, holes；Powder prepared by XRD figure spectrum display is completely amorphous state.
Amorphous powder being passivated and insulating wrapped processes, Passivation Treatment: poured into by amorphous powder in the Phosphating Solution of 1wt%, at the uniform velocity stirring is until drying；Insulating wrapped: joined by the amorphous powder after Passivation Treatment in the polyamide acetone soln of 1wt% epoxy resin and 1wt%, at the uniform velocity stirring is to dry.After insulating wrapped, through the screen cloth rescreening of 100 orders, the powder particle collecting below 100 orders is pressed.
Powder particle is put in hydraulic forming machine, use 20t/cm2Pressure be pressed into external diameter 20.3mm, internal diameter 12.7mm, be highly 6.35mm(Φ 20.3 × 12.7 × 6.35mm) annular powder core, the dwell time is 10s, and after molding, the surface composition of powder core is uniform, no significant defect.After the powder core of described molding carries out the annealing of 1 hour at 500 DEG C, it is thus achieved that iron based nano crystal powder core, detecting through XRD, Crystallization Phases is single α-Fe phase.Measure the performances such as the pcrmeability of powder core, loss and direct current biasing respectively.
After tested, powder core pcrmeability under 1MHz frequency is 67, and meanwhile, frequency stability is excellent；The loss of powder core is very low, and when 50kHz, 0.1T, loss is 745mW/cm3；Under 100Oe externally-applied magnetic field, pcrmeability remains to be maintained at 62% when not adding magnetic field.Visible, prepared new iron-based nanocrystalline magnetic core excellent combination property.
Comparative example 1:
Foundry alloy heating is melted to more than fusing point 200 DEG C and is incubated 15 minutes, aerosolization method is adopted to prepare FeSiBPNbCu alloy powder, the pressure of aerosolization is 10MPa, nozzle diameter is 1mm, by alloy powder in vacuum drying oven dried, with 200 eye mesh screens, powder is sieved, obtain target powder, SEM collection of illustrative plates display powder presents spherical, and smooth surface, without defects such as obvious hole, holes；Powder prepared by XRD figure spectrum display is completely amorphous state.
Amorphous powder being passivated and insulating wrapped processes, Passivation Treatment: poured into by amorphous powder in the Phosphating Solution of 1wt%, at the uniform velocity stirring is until drying；Insulating wrapped: joined by the amorphous powder after Passivation Treatment in the polyamide acetone soln of 1wt% epoxy resin and 1wt%, at the uniform velocity stirring is to dry.After insulating wrapped, through the screen cloth rescreening of 100 orders, the powder particle collecting below 100 orders is pressed.
Powder particle is put in hydraulic forming machine, use 18t/cm2Pressure be pressed into external diameter 20.3mm, internal diameter 12.7mm, be highly 6.35mm(Φ 20.3 × 12.7 × 6.35mm) annular powder core, the dwell time is 10s, and after molding, the surface composition of powder core is uniform, no significant defect.After the powder core of described molding is carried out at 530 DEG C the annealing of 1 hour, it is thus achieved that iron based nano crystal powder core, detect through XRD, Crystallization Phases except α-Fe mutually except, there is also Fe3(B, P) phase, makes the magnetic property of nanocrystalline magnetic core worsen.Measure the performances such as the pcrmeability of powder core, loss and direct current biasing respectively.
After tested, powder core pcrmeability under 1MHz frequency is 30；The loss of powder core is very low, and when 20kHz, 0.1T, loss is 6000mW/cm3.Visible, due to the difference of crystallization temperature, cause prepared iron based nano crystal powder core magnetic property severe exacerbation.
Technical scheme has been described in detail by embodiment described above; it it should be understood that and the foregoing is only specific embodiments of the invention; it is not limited to the present invention; all make in the spirit of the present invention any amendment, supplement or equivalent replacement etc., should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of an iron based nano crystal powder core, it is characterised in that comprise the steps:
(1) to the Composition of Fe-Based Amorphous Alloy with large-amorphous forming capacity, aerosolization method is adopted to prepare Fe-based amorphous alloy powder；
(2) the Fe-based amorphous alloy powder of target grain size is obtained by screening after the Fe-based amorphous alloy powder of preparation being processed；
(3) adopt passivator to be passivated processing to the Fe-based amorphous alloy powder after screening, then use insulating compound and binding agent that the Fe-based amorphous alloy powder after Passivation Treatment is carried out insulating wrapped process；
(4) by after the Fe-based amorphous alloy powder pressing forming handled well, annealing is carried out, it is thus achieved that iron based nano crystal powder core.
2. the preparation method of iron based nano crystal powder core according to claim 1, it is characterized in that, the mass percent of each element in the Composition of Fe-Based Amorphous Alloy of large-amorphous forming capacity that has in described step (1) is 4.5 ~ 5.5%Si, 2 ~ 4%B, 2.5 ~ 4%P, 1.5 ~ 2.5%Nb, 0.5 ~ 1%Cu, surplus is Fe.
3. the preparation method of iron based nano crystal powder core according to claim 1, it is characterized in that, in described step (1), before adopting aerosolization method to prepare Fe-based amorphous alloy powder, the Composition of Fe-Based Amorphous Alloy with large-amorphous forming capacity is heated to more than fusing point 150 ~ 300 DEG C, and is incubated 10 ~ 30min.
4. the preparation method of iron based nano crystal powder core according to claim 1, it is characterised in that it is 5 ~ 15MPa that the aerosolization method in described step (1) prepares the atomizing pressure of Fe-based amorphous alloy powder, and melt nozzle diameter is 0.5 ~ 3mm.
5. the preparation method of iron based nano crystal powder core according to claim 1, it is characterised in that in described step (2), the Fe-based amorphous alloy powder of target grain size is the powder by 200 eye mesh screens, and namely powder diameter is less than 75 μm.
6. the preparation method of iron based nano crystal powder core according to claim 1, it is characterised in that in described step (3), passivator is Phosphating Solution, and described insulating compound is mica powder, and described binding agent is epoxy resin or polyamide.
7. the preparation method of iron based nano crystal powder core according to claim 1, it is characterised in that pressure compressing in described step (4) is 10 ~ 26t/cm2, the dwell time is 5 ~ 30s.
8. the preparation method of iron based nano crystal powder core according to claim 1, it is characterised in that in described step (4), the temperature of annealing is 460 ~ 530 DEG C, and the process time is 0.5 ~ 3 hour.
9. the preparation method of iron based nano crystal powder core according to claim 1, it is characterised in that in described step (4), the atmosphere of subsequent annealing can be the reducing atmospheres such as the protective atmosphere such as nitrogen, argon or hydrogen.
10. the preparation method of iron based nano crystal powder core according to claim 6, it is characterized in that, in described step (3), processing procedure to Fe-based amorphous alloy powder is joined by Fe-based amorphous alloy powder in the Phosphating Solution of 1 ~ 10%, it is evenly stirred until dry, subsequently by the Muscovitum Homogeneous phase mixing of the Fe-based amorphous alloy powder after Passivation Treatment and 1 ~ 5%, obtain mixed-powder, finally, mixed-powder is joined in the epoxy resin of 1 ~ 5% or the acetone soln of polyamide, be evenly stirred until dry.
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