CN108172359A - Spherical iron based amorphous alloy powder and preparation method thereof and the application in amorphous powder core is prepared - Google Patents
Spherical iron based amorphous alloy powder and preparation method thereof and the application in amorphous powder core is prepared Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 210
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 49
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 39
- 239000000956 alloy Substances 0.000 claims abstract description 39
- 238000009689 gas atomisation Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 238000002161 passivation Methods 0.000 claims description 18
- 238000000137 annealing Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 238000000465 moulding Methods 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 12
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- 238000012387 aerosolization Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000010445 mica Substances 0.000 claims description 8
- 229910052618 mica group Inorganic materials 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000000443 aerosol Substances 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 16
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000011162 core material Substances 0.000 description 91
- 238000001228 spectrum Methods 0.000 description 14
- 230000007547 defect Effects 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 239000006247 magnetic powder Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 230000036961 partial effect Effects 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- 239000005300 metallic glass Substances 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 3
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15358—Making agglomerates therefrom, e.g. by pressing
- H01F1/15366—Making agglomerates therefrom, e.g. by pressing using a binder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15383—Applying coatings thereon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation methods of spherical iron based amorphous alloy powder, using the Fe-based amorphous alloy with large-amorphous forming capacity as raw material, are prepared through gas atomization；The atomic percent composition of Fe-based amorphous alloy with large-amorphous forming capacity is Fe100‑a‑b‑c‑d‑eSiaBbPcNbdCue, wherein, it be 7~11, c be 3~6, d be 0~3, e is 0~2 that a, which is 7~10, b,.The present invention provides a kind of methods that spherical iron based amorphous alloy powder is prepared by gas atomization, obtain regular appearance, uniform particle diameter, and are the spherical alloy powder of completely amorphous state.The amorphous powder core prepared using the spherical iron based amorphous alloy powder as raw material has even tissue, high intensity, high-compactness and the constant advantage of magnetic conductivity.
Description
Technical field
The invention belongs to field of magnetic material, and in particular to a kind of spherical iron based amorphous alloy powder and preparation method thereof and
Application in amorphous powder core is prepared.
Background technology
Iron base amorphous magnetically-soft alloy is with saturation induction density is high, initial permeability is high, coercivity is small, loss is low excellent
Point has excellent soft magnet performance with the iron core that the amorphous band that quick quenching technique is prepared turns to after appropriate heat treatment,
The fields such as all kinds of transformers, sensor, Switching Power Supply are widely used.But with electron electric power industrial expansion, electricity
Sub- device develops to miniaturization, high frequency and high current direction, and band is lost very around the soft magnet core of, lamination in high-frequency work
Greatly, its application in high frequency is limited.At this time, it may be necessary to work requirements are met using powder core.Powder core is using powder
Metallurgical technology is formed by soft-magnetic alloy powder and dielectric mixing compacting.Traditional powder core mainly has ferrocart core, iron silicon
Powder core, iron Si-Al Magnetic Powder Core, iron nickel powder core and FeNiCo magnetic core etc..Ferrocart core is cheap, but high frequency characteristics and loss characteristic are not
It is good；Iron silica flour core is moderate, DC stacked to have excellent performance, but high-frequency loss is high；Iron Si-Al Magnetic Powder Core wide application, loss is low,
Frequency performance is good, has excellent cost performance, but DC superposition characteristic is not ideal enough；Iron nickel powder core has best D.C. magnetic biasing
Characteristic, but higher price, loss are also high；Iron nickel molybdenum best performance is got over, but also most expensive, fancy price limit price
Its application range.
Fe-based amorphous powder core has the spies such as permanent magnetic conductivity, high resistivity, low-loss, temperature stability be good in high frequency
Point, and it is of low cost, it is the important development direction of magnetic powder core material, is increasingly becoming the hot spot of research and application in recent years.Fu Min
Deng (Arms Material scientific and engineering, 2014,37:90) passivator, insulating compound and the binding agent in insulating wrapped technique are had studied
The influence of FeSiB amorphous powder core performances is crushed to band, result of study shows the Effective permeability of powder core with insulating wrapped
The increase of agent content and reduce, quality factor q increases with the increase of additive amount, and the mass fraction of passivator is 4%~8%
When, powder core is had excellent performance, and magnetic conductivity reaches 45.Tang Jian etc. (functional material, 2012,43:96.) heat treatment temperature pair is had studied
Fe78Si9B13The affecting laws of amorphous powder core performance, the results showed that, under conditions of less than starting crystallization temperature, amorphous magnetic powder
The loss of core shows increased trend after first reducing with the raising of annealing temperature, and magnetic conductivity shows opposite trend.
When heat treatment temperature is excessively high, crystallization occurs for amorphous magnetic powder, and magnetic anisotropy constant increases, and magnetic conductivity is caused drastically to decline, and magnetic
Conductance changes less in the range of 3MHz, and frequency stability is good.Application No. is 201310018768.7 patent of invention announcements
A kind of preparation method of magnetically soft alloy powder core including amorphous band embrittlement processing, is ground into powder, screening and proportioning, blunt
Change processing and insulating wrapped, compression moulding, annealing and spraying, the high frequency performance of powder core is excellent.Application No. is
201410394382.0 patent of invention disclose a kind of preparation method of amorphous metal soft magnetic-powder core, by amorphous metal soft magnet powder
End carries out mixing by obtaining two kinds of different powder of particle diameter distribution after the screening of the sieves of different sieve meshes and reaches powder, it is re-compacted into
Type carries out isostatic pressed processing, and under the conditions of being 300-450 DEG C in temperature answer after obtaining amorphous metal soft magnetic-powder core green compact
Power makes annealing treatment, and obtains the amorphous metal soft magnetic-powder core that density is high and is evenly distributed.
However, used by above-mentioned article and amorphous powder core involved in patent magnetic powder be by band crush method come
It preparing, impurity is readily incorporated during ball mill crushing, the component for leading to powder is uneven, meanwhile, the powder obtained
The mostly sheet with corner angle, it is difficult to insulate, the loss for leading to powder core is higher, and anti-direct current biasing ability is poor.
Invention content
The present invention provides a kind of methods that spherical iron based amorphous alloy powder is prepared by gas atomization, obtain pattern
Regular, uniform particle diameter, and be the spherical alloy powder of completely amorphous state.It is prepared by raw material of the spherical iron based amorphous alloy powder
Amorphous powder core there is even tissue, high intensity, high-compactness and the constant advantage of magnetic conductivity.
Specific technical solution is as follows：
A kind of preparation method of spherical iron based amorphous alloy powder, with the Fe-based amorphous alloy with large-amorphous forming capacity
For raw material, it is prepared through gas atomization；
The atomic percent composition of the Fe-based amorphous alloy with large-amorphous forming capacity is Fe100-a-b-c-d- eSiaBbPcNbdCue, wherein, it be 7~11, c be 3~6, d be 0~3, e is 0~2 that a, which is 7~10, b,.
Preferably, the gas atomization is specially：
Under air or oxygen atmosphere, Fe-based amorphous alloy is heated and melts and keeps the temperature, to improve fluidity of molten with reality
Existing excellent atomizing effect, it is desirable to provide certain degree of superheat, it is non-with reference to the composition characteristic of series alloy in the present invention and guarantee
The starting point of brilliant Forming ability, preferably, Fe-based amorphous alloy is heated to more than its fusing point 150~300 DEG C and heat preservation 10
~30min.Further preferably：Fe-based amorphous alloy is heated to more than its fusing point 200~250 DEG C and 15~25min of heat preservation.
The aerosolization pressure is 5~15MPa, further preferably 9~11MPa.
Under above-mentioned preferred process conditions, further preferably, the Fe-based amorphous conjunction with large-amorphous forming capacity
Gold is selected from Fe76Si9B10P5Alloy, (Fe0.76Si0.09B0.1P0.05)99Nb1Alloy, (Fe0.76Si0.09B0.1P0.05)98.5Nb1Cu0.5It closes
Gold or (Fe0.76Si0.09B0.1P0.05)98.25Nb1Cu0.75Alloy.
It is found through experiment that above-mentioned preferred four kinds of Fe-based amorphous alloys are respectively provided with splendid amorphous formation ability, it is screened
Low, magnetic conductivity conservation rate height is lost in the amorphous powder core prepared after to target grain size.
Further, with (Fe0.76Si0.09B0.1P0.05)99Nb1Alloy is raw material, and the grain size being prepared is less than 100 μm
Alloy powder is completely amorphous state, further improves the utilization rate of the alloy raw material.
Further, with (Fe0.76Si0.09B0.1P0.05)98.5Nb1Cu0.5Alloy or (Fe0.76Si0.09B0.1P0.05)98.25Nb1Cu0.75Alloy is raw material, and the amorphous powder core that the alloy powder being prepared makes has lower loss, higher
Magnetic conductivity conservation rate.
It is found through experiment that using above-mentioned preferred four kinds of Fe-based amorphous alloys, and the processing parameter setting of aerosolization is existed
In above-mentioned preferred scope, the alloy powder pattern that is prepared is mostly that regular spherical shape, particle diameter distribution are more concentrated, and be complete
Amorphous state.
The invention also discloses the spherical iron based amorphous alloy powder prepared according to the above method, grain size is -150 mesh, is
Completely amorphous state.
The invention also discloses application of the above-mentioned spherical iron based amorphous alloy powder in amorphous powder core is prepared, specifically
For：
By the spherical iron based amorphous alloy powder be passivated successively with insulating wrapped processing, then it is repressed molding and
The amorphous powder core is obtained after annealing.
Preferably, the passivation and insulating wrapped processing, specially：
(1) spherical iron based amorphous alloy powder with phosphating solution is mixed, is evenly stirred until drying, the alloy after being passivated
Powder；
The phosphating solution quality is the 1~5% of spherical iron based amorphous alloy powder quality；
The main component of phosphating solution is dihydric phosphate, such as Zn (H2PO4)2And suitable free phosphoric acid and accelerator etc..
(2) alloy powder after passivation in step (1) with mica, binding agent is mixed, is evenly stirred until drying；
In terms of the alloy powder quality after passivation, the addition of the mica is 1~5%, the addition of the binding agent
It is 1~4%；
The binding agent is selected from the epoxy resin/acetone soln or polyamide resin that mass percent concentration is 1~5%
Fat/acetone soln.
Preferably, the pressure of the compression moulding is 10~26t/cm2, the dwell time is 5~120s；
The annealing carries out under protective atmosphere or reducing atmosphere, and the temperature of annealing is 300~450 DEG C,
Time is 0.5~3h.
Compared with prior art, the present invention has the advantages that：
1st, the present invention is prepared spherical using the Fe-based amorphous alloy with large-amorphous forming capacity as raw material using gas atomization
Fe-based amorphous alloy powder can avoid being mixed into impurity existing for conventional tape crush method, uneven components and there are sharp corners
The problem of, conducive to the insulating wrapped of powder, so as to reduce the core loss of powder core, improve its anti-direct current biasing ability.
2nd, the present invention is with the raw material of above-mentioned spherical iron based amorphous alloy powder, then passes through compression moulding and stress relief annealing
After processing, even tissue, high intensity, high-compactness and the constant Fe-based amorphous powder core of magnetic conductivity have been obtained, has been expected to be used as each
The various inductance elements such as filtering, current stabilization and energy storage on kind switch power module.
Description of the drawings
Fig. 1 is the SEM figures of the spherical iron based amorphous alloy powder prepared in embodiment 1；
Fig. 2 is the XRD spectrum of spherical iron based amorphous alloy powder prepared in embodiment 1；
Fig. 3 be in embodiment 1 the amorphous powder core magnetic conductivity for preparing with the variation tendency of frequency；
Fig. 4 be in embodiment 1 the amorphous powder core core loss for preparing with the variation tendency of frequency；
Fig. 5 be in embodiment 1 magnetic conductivity of amorphous powder core for preparing with the variation tendency of externally-applied magnetic field；Fig. 6 is implements
The XRD spectrum of spherical iron based amorphous alloy powder that example 2~5 is prepared respectively.
Specific embodiment
The method for preparing new iron-based amorphous powder core is illustrated below according to the preferred embodiment of the present invention.
Embodiment 1
Master alloy under atmospheric environment is heated and melts to 200 DEG C of more than fusing point and keeps the temperature 10 minutes, using gas atomization
Prepare Fe76Si9B10P5Alloy powder, the pressure of aerosolization are 10MPa, nozzle diameter 1mm, with 200 mesh screens to powder into
Row screening, obtains target powder, the pattern of target powder is analyzed with scanning electron microscope (SEM), as shown in Figure 1,
As can be seen that powder shows spherical shape, surface is smooth, the defects of without apparent hole, hole；It is detected with X-ray diffractometer (XRD)
Structure, the results are shown in Figure 2, it can be seen that does not have any corresponding diffraction maximum of crystallization in XRD spectrum, only there are one wide
Diffusing scattering peak illustrates that prepared powder is completely amorphous state.
Amorphous powder is passivated and insulating wrapped processing, amorphous powder is added to phosphating solution, and (phosphating solution quality is
The 2% of amorphous powder quality) in, it is evenly stirred until drying, the powder after passivation is then added to by the powder after being passivated
In the mixed solution of mica and epoxy resin/acetone soln (in terms of the powder quality after passivation, the quality for adding in mica is 1%,
2%) quality of epoxy resin/acetone soln is, is evenly stirred until drying.After insulating wrapped, by 100 mesh sieve again
Screening is collected the powder particle below 100 mesh and is pressed.
Powder particle is put into hydraulic forming machine, uses 18t/cm2Pressure be pressed into outer diameter 20.3mm, internal diameter
12.7mm, the highly annular powder core for 6.35mm (20.3 × 12.7 × 6.35mm of Φ), dwell time 30s, magnetic after molding
The surface composition of powder core is uniform, no significant defect.The destressing of 1 hour is carried out at 400 DEG C to the molding powder core
After annealing, Fe-based amorphous powder core is obtained, measures the performances such as magnetic conductivity, loss and the direct current biasing of powder core respectively.
After tested, magnetic conductivity of the powder core under 1MHz frequencies is 69, meanwhile, frequency stability is excellent, as shown in Figure 3；
The loss of powder core is very low, under the conditions of 50kHz, 0.1T, is lost as 707mW/cm3, as shown in Figure 4；In 100Oe externally-applied magnetic fields
Under, magnetic conductivity remains to be maintained at 61% when not adding magnetic field, as shown in Figure 5, it is seen then that prepared new iron-based amorphous powder core
Excellent combination property.
Embodiment 2~5
The preparation process of spherical iron based amorphous alloy powder and amorphous powder core and 1 all same of embodiment, differ only in：
The gas atomization of spherical iron based amorphous alloy powder is prepared, is carried out under different partials pressure of oxygen.Embodiment is set forth in Fig. 6
2 (partial pressure of oxygen be 3 × 104Pa), (partial pressure of oxygen is 5 × 10 to embodiment 34Pa), (partial pressure of oxygen is 7 × 10 to embodiment 44Pa) and implement
(partial pressure of oxygen is 9 × 10 to example 54Pa the XRD spectrum of -200 mesh powder) prepared respectively, as shown in the figure, (real when partial pressure of oxygen is relatively low
Apply example 2), there is apparent crystallization in the powder of preparation, and with the raising (embodiment 3~5) of partial pressure of oxygen, it can obtain completely
The spherical powder of amorphous -200 mesh.
Embodiment 6
Master alloy heating is melted to more than fusing point 150 DEG C and keeps the temperature 15 minutes, is prepared using gas atomization
Fe76Si9B10P5Alloy powder, the pressure of aerosolization is 9MPa, and nozzle diameter 1mm sieves powder with 100 mesh screens
Point, target powder is obtained, SEM spectrum shows that powder shows spherical shape, and surface is smooth, the defects of without apparent hole, hole；XRD diagram
The prepared powder of spectrum display is completely amorphous state.
Amorphous powder is passivated and insulating wrapped processing, amorphous powder is added to phosphating solution, and (phosphating solution quality is
The 2% of amorphous powder quality) in, it is evenly stirred until drying, the powder after passivation is then added to by the powder after being passivated
In the mixed solution of mica and epoxy resin/acetone soln (in terms of the powder quality after passivation, the quality for adding in mica is 2%,
2%) quality of epoxy resin/acetone soln is, is evenly stirred until drying.After insulating wrapped, by 100 mesh sieve again
Screening is collected the powder particle below 100 mesh and is pressed.
Powder particle is put into hydraulic forming machine, uses 16t/cm2Pressure be pressed into outer diameter 20.3mm, internal diameter
12.7mm, the highly annular powder core for 6.35mm (20.3 × 12.7 × 6.35mm of Φ), dwell time 20s, magnetic after molding
The surface composition of powder core is uniform, no significant defect.The destressing of 1 hour is carried out at 400 DEG C to the molding powder core
After annealing, Fe-based amorphous powder core is obtained, measures the performances such as magnetic conductivity, loss and the direct current biasing of powder core respectively.
After tested, magnetic conductivity of the powder core under 1MHz frequencies is 63, meanwhile, frequency stability is excellent；The damage of powder core
Consumption is very low, under the conditions of 50kHz, 0.1T, is lost as 900mW/cm3；Under 100Oe externally-applied magnetic fields, magnetic conductivity remains to be maintained at
Not plus 63% during magnetic field.As it can be seen that prepared new iron-based amorphous powder core excellent combination property.
Embodiment 7
Master alloy heating is melted to more than fusing point 200 DEG C and keeps the temperature 20 minutes, is prepared using gas atomization
(Fe0.76Si0.09B0.1P0.05)99Nb1Alloy powder, the pressure of aerosolization is 9MPa, nozzle diameter 1.3mm, by alloy powder
In vacuum drying chamber after drying, powder is sieved with 200 mesh screens, obtains target powder, SEM spectrum shows that powder is in
Reveal spherical shape, surface is smooth, the defects of without apparent hole, hole；XRD spectrum shows that prepared powder is completely amorphous state.
Amorphous powder is passivated and insulating wrapped is handled, Passivation Treatment：Amorphous powder is poured into the phosphating solution of 1wt%
In, at the uniform velocity stirring is until dry；Insulating wrapped：Amorphous powder after Passivation Treatment is added to 1wt% epoxy resin and 1wt%
Polyamide acetone soln in, at the uniform velocity stir to drying.After insulating wrapped, by the sieve rescreening of 100 mesh, receive
Collect the powder particle below 100 mesh to be pressed.
Powder particle is put into hydraulic forming machine, uses 18t/cm2Pressure be pressed into outer diameter 20.3mm, internal diameter
12.7mm, the highly annular powder core for 6.35mm (20.3 × 12.7 × 6.35mm of Φ), dwell time 15s, magnetic after molding
The surface composition of powder core is uniform, no significant defect.At the annealing for carrying out 1 hour at 450 DEG C to the molding powder core
After reason, Fe-based amorphous powder core is obtained, measures the performances such as magnetic conductivity, loss and the direct current biasing of powder core respectively.
After tested, magnetic conductivity of the powder core under 1MHz frequencies is 65, meanwhile, frequency stability is excellent；The damage of powder core
Consumption is very low, under the conditions of 50kHz, 0.1T, is lost as 670mW/cm3；Under 100Oe externally-applied magnetic fields, magnetic conductivity remains to be maintained at
Not plus 63% during magnetic field.As it can be seen that prepared new iron-based amorphous powder core excellent combination property.
Embodiment 8
Master alloy heating is melted to more than fusing point 250 DEG C and keeps the temperature 15 minutes, is prepared using gas atomization
(Fe0.76Si0.09B0.1P0.05)99Nb1Alloy powder, the pressure of aerosolization is 11MPa, nozzle diameter 1mm, with 200 mesh screens
Powder is sieved, obtains target powder, SEM spectrum shows that powder shows spherical shape, and surface is smooth, without apparent hole, hole
The defects of；XRD spectrum shows that prepared powder is completely amorphous state.
Amorphous powder is passivated and insulating wrapped is handled, Passivation Treatment：Amorphous powder is poured into the phosphating solution of 1wt%
In, at the uniform velocity stirring is until dry；Insulating wrapped：Amorphous powder after Passivation Treatment is added to 2wt% epoxy resin and 1wt%
Polyamide acetone soln in, at the uniform velocity stir to drying.After insulating wrapped, by the sieve rescreening of 100 mesh, receive
Collect the powder particle below 100 mesh to be pressed.
Powder particle is put into hydraulic forming machine, uses 17t/cm2Pressure be pressed into outer diameter 20.3mm, internal diameter
12.7mm, the highly annular powder core for 6.35mm (20.3 × 12.7 × 6.35mm of Φ), dwell time 10s, magnetic after molding
The surface composition of powder core is uniform, no significant defect.The destressing of 1 hour is carried out at 420 DEG C to the molding powder core
After annealing, Fe-based amorphous powder core is obtained, measures the performances such as magnetic conductivity, loss and the direct current biasing of powder core respectively.
After tested, magnetic conductivity of the powder core under 1MHz frequencies is 63, meanwhile, frequency stability is excellent；The damage of powder core
Consumption is very low, under the conditions of 50kHz, 0.1T, is lost as 680mW/cm3；Under 100Oe externally-applied magnetic fields, magnetic conductivity remains to be maintained at
Not plus 62% during magnetic field.As it can be seen that prepared new iron-based amorphous powder core excellent combination property.
Embodiment 9
Master alloy heating is melted to more than fusing point 200 DEG C and keeps the temperature 15 minutes, is prepared using gas atomization
(Fe0.76Si0.09B0.1P0.05)98.5Nb1Cu0.5Alloy powder, the pressure of aerosolization is 10MPa, nozzle diameter 1mm, with 200 mesh
Sieve sieves powder, obtains target powder, and SEM spectrum shows that powder shows spherical shape, and surface is smooth, without apparent
The defects of hole, hole；XRD spectrum shows that prepared powder is completely amorphous state.
Amorphous powder is passivated and insulating wrapped is handled, Passivation Treatment：Amorphous powder is poured into the phosphating solution of 1wt%
In, at the uniform velocity stirring is until dry；Insulating wrapped：It is molten that amorphous powder after Passivation Treatment is added to 2wt% epoxy resin acetone
In liquid, at the uniform velocity stir to drying.After insulating wrapped, by the sieve rescreening of 100 mesh, the powder below 100 mesh is collected
Particle is pressed.
Powder particle is put into hydraulic forming machine, uses 20t/cm2Pressure be pressed into outer diameter 20.3mm, internal diameter
12.7mm, the highly annular powder core for 6.35mm (20.3 × 12.7 × 6.35mm of Φ), dwell time 30s, magnetic after molding
The surface composition of powder core is uniform, no significant defect.The destressing of 1 hour is carried out at 400 DEG C to the molding powder core
After annealing, Fe-based amorphous powder core is obtained, measures the performances such as magnetic conductivity, loss and the direct current biasing of powder core respectively.
After tested, magnetic conductivity of the powder core under 1MHz frequencies is 65, meanwhile, frequency stability is excellent；The damage of powder core
Consumption is very low, under the conditions of 100kHz, 0.05T, is lost as 450mW/cm3；Under 100Oe externally-applied magnetic fields, magnetic conductivity remains to keep
69% when not adding magnetic field.As it can be seen that prepared new iron-based amorphous powder core excellent combination property.
Embodiment 10
Master alloy heating is melted to more than fusing point 200 DEG C and keeps the temperature 15 minutes, is prepared using gas atomization
(Fe0.76Si0.09B0.1P0.05)98.25Nb1Cu0.75Alloy powder, the pressure of aerosolization is 9MPa, nozzle diameter 1.2mm, is used
200 mesh screens sieve powder, obtain target powder, and SEM spectrum shows that powder shows spherical shape, and surface is smooth, without bright
The defects of aobvious hole, hole；XRD spectrum shows that prepared powder is completely amorphous state.
Amorphous powder is passivated and insulating wrapped is handled, Passivation Treatment：Amorphous powder is poured into the phosphating solution of 1wt%
In, at the uniform velocity stirring is until dry；Insulating wrapped：Amorphous powder after Passivation Treatment is added to 1wt% epoxy resin and 1wt%
Polyamide acetone soln in, at the uniform velocity stir to drying.After insulating wrapped, by the sieve rescreening of 100 mesh, receive
Collect the powder particle below 100 mesh to be pressed.
Powder particle is put into hydraulic forming machine, uses 18t/cm2Pressure be pressed into outer diameter 20.3mm, internal diameter
12.7mm, the highly annular powder core for 6.35mm (20.3 × 12.7 × 6.35mm of Φ), dwell time 10s, magnetic after molding
The surface composition of powder core is uniform, no significant defect.The destressing of 1 hour is carried out at 420 DEG C to the molding powder core
After annealing, Fe-based amorphous powder core is obtained, measures the performances such as magnetic conductivity, loss and the direct current biasing of powder core respectively.
After tested, magnetic conductivity of the powder core under 1MHz frequencies is 73；The loss of powder core is very low, in 100kHz, 0.05T
Under the conditions of, it is lost as 420mW/cm3, under 100Oe externally-applied magnetic fields, magnetic conductivity remains to be maintained at 66% when not adding magnetic field.It can
See, prepared new iron-based amorphous powder core excellent combination property.
Technical scheme of the present invention is described in detail in embodiment described above, and the foregoing is merely the present invention's
Specific embodiment is not intended to restrict the invention, all any modifications made in the spirit of the present invention, supplement or equivalent
Replace etc., it should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of spherical iron based amorphous alloy powder, which is characterized in that with the iron with large-amorphous forming capacity
Base noncrystal alloy is raw material, is prepared through gas atomization；
The atomic percent composition of the Fe-based amorphous alloy with large-amorphous forming capacity is Fe100-a-b-c-d- eSiaBbPcNbdCue, wherein, it be 7~11, c be 3~6, d be 0~3, e is 0~2 that a, which is 7~10, b,.
2. the preparation method of spherical iron based amorphous alloy powder according to claim 1, which is characterized in that the aerosol
Change method is specially：
Under air or oxygen atmosphere, Fe-based amorphous alloy is heated and melts and keeps the temperature, and control the pressure of aerosolization for 5~
15MPa most obtains the spherical iron based amorphous alloy powder after drying, screening afterwards.
3. the preparation method of spherical iron based amorphous alloy powder according to claim 2, which is characterized in that will be Fe-based amorphous
Alloy is heated to more than its fusing point 150~300 DEG C and 10~30min of heat preservation.
4. the preparation method of spherical iron based amorphous alloy powder according to claim 3, which is characterized in that will be Fe-based amorphous
Alloy is heated to more than its fusing point 200~250 DEG C and 15~25min of heat preservation.
5. according to the preparation method of any spherical iron based amorphous alloy powder of Claims 1 to 4, which is characterized in that institute
It states the Fe-based amorphous alloy with large-amorphous forming capacity and is selected from Fe76Si9B10P5Alloy, (Fe0.76Si0.09B0.1P0.05)99Nb1It closes
Gold, (Fe0.76Si0.09B0.1P0.05)98.5Nb1Cu0.5Alloy or (Fe0.76Si0.09B0.1P0.05)98.25Nb1Cu0.75Alloy.
6. a kind of spherical iron based amorphous alloy powder prepared according to any method of Claims 1 to 5, feature exist
In the grain size of the spherical iron based amorphous alloy powder is -150 mesh, is completely amorphous state.
7. a kind of application of spherical iron based amorphous alloy powder according to claim 6 in amorphous powder core is prepared,
It is characterized in that, specially：
The spherical iron based amorphous alloy powder is passivated and insulating wrapped processing, then repressed molding and annealing successively
The amorphous powder core is obtained after processing.
8. application of the spherical iron based amorphous alloy powder according to claim 7 in amorphous powder core is prepared, feature
It is, the passivation and insulating wrapped processing, specially：
(1) spherical iron based amorphous alloy powder with phosphating solution is mixed, is evenly stirred until drying, the alloyed powder after being passivated
End；
The phosphating solution quality is the 1~5% of spherical iron based amorphous alloy powder quality；
(2) alloy powder after passivation in step (1) with mica, binding agent is mixed, is evenly stirred until drying；
In terms of the alloy powder quality after passivation, the addition of the mica is 1~5%, and the addition of binding agent is 1~4%；
The binding agent is selected from the epoxy resin/acetone soln or polyamide/the third that mass percent concentration is 1~5%
Ketone solution.
9. application of the spherical iron based amorphous alloy powder according to claim 7 in amorphous powder core is prepared, feature
It is, the pressure of the compression moulding is 10~26t/cm2, the dwell time is 5~120s.
10. application of the spherical iron based amorphous alloy powder according to claim 7 in amorphous powder core is prepared, feature
It is, the annealing carries out under protective atmosphere or reducing atmosphere, and the temperature of annealing is 300~450 DEG C, the time
For 0.5~3h.
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