CN105945294A - Iron-silicon-chromium soft magnetic powder, preparation method and application thereof - Google Patents
Iron-silicon-chromium soft magnetic powder, preparation method and application thereof Download PDFInfo
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- CN105945294A CN105945294A CN201610384098.4A CN201610384098A CN105945294A CN 105945294 A CN105945294 A CN 105945294A CN 201610384098 A CN201610384098 A CN 201610384098A CN 105945294 A CN105945294 A CN 105945294A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- H—ELECTRICITY
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- 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
- H01F1/14766—Fe-Si based alloys
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- 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
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- 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
- B22F2009/084—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 combination of methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention discloses iron-silicon-chromium soft magnetic powder, a preparation method and application thereof. The preparation method comprises the following steps: 1) iron-silicon-chromium soft magnetic alloy powder raw materials are added in a medium-frequency induction furnace for atmospheric smelting to obtain alloy liquid; and 2) under the condition of nitrogen protection, the alloy liquid is fed in an atomization tower; in the feeding process, two atomization mediums of ultrahigh-pressure atomization water and low-pressure vortex gas synchronously acts on the alloy liquid; and the alloy liquid is strongly crushed as a lot of fine metal molten drops, and is cooled and condensed as the iron-silicon-chromium soft magnetic alloy powder. The iron-silicon-chromium soft magnetic powder with high loose packing density, high tap density, low oxygen content and higher inductance value and magnetic conductivity can be prepared; and the iron-silicon-chromium soft magnetic powder can serve as a raw material of a micro inductor, and is widely applied.
Description
Technical field
The present invention relates to soft-magnetic alloy powder technical field, specifically refer to a kind of ferrum silicochromium soft magnetic powder
Preparation method and applications.
Background technology
Metal soft magnetic alloy powder body material is that in magnetic material, purposes is the widest, the class material that consumption is maximum.
Inductance primarily serve in circuit filtering, vibrate, postpone, the effect such as trap, also screen signal,
Cross the effects such as noise filtering, stabling current and suppression Electromagnetic Interference.Therefore miniature inductance has become as height
Primary Component particularly important in end electronic manufacturing industry.Along with automated control technology, intelligent terminal
Deng the progress of electronic manufacturing field, electronic device is day by day to miniaturization, high-performance, high speed development.
This just promotes soft magnetic materials to develop to ultra-fine, high magnetic permeability and low-loss further.Main gold
Belonging to soft-magnetic alloy powder preparation method is chemical reaction method, melt atomization method, mechanical crushing method and electrolysis
Sedimentation etc..Wherein, melt atomization method is prepared alloy powder and is had identical with set molten alloy
Chemical composition, also there is typical rapid solidification structure, alloy component range width, powder morphology ball
Shape degree is good, the feature that particle size distribution is wide.
At present, by above-mentioned atomization produce for ring-shaped inductors ferrum silicochromium soft magnetic powder, it is deposited
Low in apparent density of powder, tap density, oxygen content in power is high, and product pressed density is low, inductance value
Low defect.In consideration of it, the problems referred to above are furtherd investigate by inventor, and a kind of ferrum is proposed
The preparation method and applications of silicochromium soft magnetic powder.
Summary of the invention
One purpose of the present invention is to provide the preparation method of a kind of ferrum silicochromium soft magnetic powder, overcomes existing
It is low to there is apparent density of powder, tap density in the ferrum silicochromium soft magnetic powder that water atomization is produced, powder oxygen
Content is high, the problem that product pressed density is low, inductance value is low.
In order to reach above-mentioned purpose, the solution of the present invention is:
A kind of preparation method of ferrum silicochromium soft magnetic powder, step is as follows:
1) adding in intermediate frequency furnace by ferrum silicochromium soft-magnetic alloy powder powder stock, air is smelted and is obtained alloy
Liquid;
2) under conditions of nitrogen is protected, aluminium alloy is sent into atomisation tower, during sending into, pass through
Supertension atomized water and lower scroll gas both atomizing mediums simultaneously act on aluminium alloy, by alloy
Liquid strength is broken into a large amount of fine metal molten drop, and cooled and solidified is ferrum silicochromium soft-magnetic alloy powder then.
Described ferrum silicochromium soft-magnetic alloy powder raw materials quality ratio is: pure chromium 3.5-6.5%, pure silicon
3.0-6.5%, silicon calcium powder 0.6-0.8%, calcium oxide 1.0-1.5%, surplus is ferrum.
Described 1), in the smelting process of step, control to smelt power 80-240KW;By pure chromium, pure silicon
And ferrum is divided into two parts, during smelting, add a pure chromium, pure silicon and ferrum prior to furnace bottom, change clear process land
Continuous another part of pure chromium, pure silicon and the residue ferrum of adding, and add before changing clearly;Control molten steel temperature >=
1580-1600 DEG C, reduce power and to 10-30KW and add silicon calcium powder and calcium oxide covering molten steel, slag making
Slagging-off, purification obtains aluminium alloy.
Described 2), in step, aluminium alloy is sent into atomisation tower and is first preliminarily formed bigger metal drop, leads to afterwards
Cross supertension atomized water and lower scroll gas both atomizing mediums simultaneously act on described in bigger metal
Molten drop, is broken into a large amount of fine metal molten drop by this bigger metal drop strength, and cooled and solidified is then
Ferrum silicochromium soft-magnetic alloy powder.
Described 2), in step, supertension atomized water adds the table of the 1-15wt% accounting for atomized water gross weight
Face activating agent.
Described surfactant is 17 alkenyl amine ethyl imidazol(e) hyamines, Polyethylene Glycol or 12
Alkyl sodium sulfate.
The pressure of described supertension atomized water is 120-150MPa.
The pressure of described lower scroll gas is 0.2-0.6Mpa.
Another object of the present invention is to provide a kind of ferrum silicochromium soft magnetic powder, this ferrum silicochromium soft magnetic powder
Prepared by the preparation method described in claim 1-8.
It is still another object of the present invention to provide the application of a kind of ferrum silicochromium soft magnetic powder, this ferrum silicochromium is soft
Magnetic powder is prepared by preparation method described in claim 1-8, using this ferrum silicochromium soft magnetic powder as
The raw material of miniature inductance.
After using such scheme, one ferrum silicochromium soft magnetic powder of the present invention, its preparation method and application thereof,
Having the beneficial effects that relative to prior art:
One, the present invention innovates the water-gas combined powder by atomization method of employing, and it combines aerosolization and water atomization
Advantage, the ferrum silicochromium soft magnetic powder of gained overcomes the ferrum silicochromium soft magnetic powder that existing water atomization is produced
There is apparent density of powder, tap density low, oxygen content in power is high, and product pressed density is low, inductance
It is worth low problem;The present invention can prepare D50=3~the multiple granularity of 10 μm, powder granule good sphericity,
Adhesion is few, and composition is uniform;
Two, further, in atomized water, add surfactant, reduce molten drop surface tension nodularization
While powder, during decreasing, the oxidation to high-temperature metal molten drop of the water decomposition oxygen, reduces further
The oxygen content of powder;Apparent density and the tap density of powder can also be effectively improved further, carry
The high pressed density of product;
Three, further, by the kind of activating agent in the present invention and the selection of proportion, can be more preferable
Ensure that the soft-magnetic alloy powder apparent density of preparation, tap density are high, oxygen content in power is low, product
Suppression performance is good, and inductance value is high.
Detailed description of the invention
Below in conjunction with detailed description of the invention, this case is described in further detail.
This case relates to the preparation method of a kind of ferrum silicochromium soft magnetic powder, and step is as follows:
1) adding in intermediate frequency furnace by ferrum silicochromium soft-magnetic alloy powder powder stock, air is smelted and is obtained alloy
Liquid;
Ferrum silicochromium soft-magnetic alloy powder powder stock can be the existing conventional raw material used, and is given and is preferable to carry out
Example, described ferrum silicochromium soft-magnetic alloy powder raw materials quality ratio is: pure chromium 3.5-6.5%, pure silicon 3.0-6.5%,
Silicon calcium powder 0.6-0.8%, calcium oxide 1.0-1.5%, surplus is ferrum.
Further, in described smelting process, control to smelt power 80-240KW;Each alloy raw material has
Having feed time and order to be particular about, such metallurgical effect is more preferably;Specifically, first by pure chromium, pure silicon
And ferrum is divided into suitable two part, during smelting, it is added thereto a appropriate pure chromium, pure silicon prior to furnace bottom
And ferrum, change clear process and add another part of pure chromium, pure silicon and residue ferrum successively, and add before changing clearly;
Afterwards, control molten steel temperature >=1580-1600 DEG C, reduce power to 10-30KW and add silicon calcium powder and
Calcium oxide covers molten steel, and slag making removes the gred, and purification obtains aluminium alloy.Described raw material is divided into suitable two part
Being not particularly limited, a preferred embodiment is to be divided into equal two part, and every part of weight is the 50% of gross weight.
2) under conditions of nitrogen is protected, aluminium alloy is sent into atomisation tower, during sending into, pass through
Supertension atomized water and lower scroll gas both atomizing mediums simultaneously act on aluminium alloy, by alloy
Liquid strength is broken into a large amount of fine metal molten drop, and cooled and solidified is ferrum silicochromium soft-magnetic alloy powder then.
The pressure of described supertension atomized water specifically controls as 120-150MPa.Described lower scroll gas
Pressure be 0.2-0.6Mpa, a preferred embodiment is 0.5MPa.
It is also preferred that the left this 2) in step, when aluminium alloy sends into atomisation tower, the Lou eye mode that first passes through flows into mist
Change tower, by its bigger metal drop of the most broken formation, afterwards by supertension atomized water and low pressure whirlpool
Rotation gas both atomizing mediums simultaneously act on described in bigger metal drop, by this bigger metal drop
Strength is broken into a large amount of fine metal molten drop, and cooled and solidified is ferrum silicochromium soft-magnetic alloy powder then.
Preferably, by 2) use vibration after the ferrum silicochromium soft-magnetic alloy powder of step gained is vacuum dried
Sieve screening, available D50=3~the multiple granularity of 10 μm.
Preferably, described 2), in step, supertension atomized water is additionally added and accounts for atomized water gross weight
The surfactant of 1-15wt%.Further, in order to reach more preferable effect, surface in described atomized water
Activating agent addition is the 5-10wt% of atomized water gross weight.Specific embodiment, this surfactant is 17
Alkenyl amine ethyl imidazol(e) hyamine (ODD), Polyethylene Glycol (PEG-600) or lauryl sulphate acid
Sodium (SDS).
The present invention, by being changed atomized water composition in the high-pressure water atomization process stage, adds table
Face activating agent in atomized water, is allowed to during high-pressure water is atomized rapid adsorption in particle surface,
Reduce oxidation, reduce system surface energy, and surfactant adsorption can cause particle surface with phase
Coulomb repulsion between same electric charge, beneficially particle, concurrently forms certain space steric effect, anti-
There is secondary agglomeration in the superfines that only atomization is formed, improves apparent density and the tap density of powder.
Meanwhile, by adding the surfactant of mentioned kind, effectively improve powder suppression performance, improve
Product pressed density and inductance value.It addition, the present invention is added activating agent to atomized water composition
Changing, it plays a role with water-gas combined atomization process is inseparable.Light water atomization starting point is too
Low, it is impossible to form powder morphology, so it is also futile for adding thing in atomized water again.
Embodiment 1
A kind of preparation method of ferrum silicochromium soft magnetic powder, step is as follows:
1) adding in intermediate frequency furnace by high-purity for ferrum silicochromium material, air is smelted;This ferrum silicon in the present embodiment
Chromium soft-magnetic alloy powder material choice is: pure chromium 3.5-6.5%, pure silicon 3.0-6.5%, silicon calcium powder
0.6-0.8%, calcium oxide 1.0-1.5%, surplus is ferrum;
In fusion process, control to smelt power 80-240KW;Alloying element feed time and order be:
Add appropriate pure chromium, pure silicon and square iron prior to furnace bottom, change clear process add successively pure chromium, pure silicon and
Residue square iron, and add before changing clearly, molten steel temperature >=1580-1600 DEG C, reduction power to 10-30KW
And adding silicon calcium powder and calcium oxide covering molten steel, slag making removes the gred, purified metal liquid (aluminium alloy);
2) under conditions of nitrogen is protected, molten metal enters atomisation tower by leakage eye and is broken into bigger metal
Molten drop, this bigger molten drop is again by the water-gas combined atomization process of the invention described above, i.e. by supertension mist
Change water and lower scroll gas both atomizing mediums simultaneously act on aluminium alloy, by broken for aluminium alloy strength
Being broken into a large amount of fine metal molten drop, cooled and solidified obtains ferrum silicochromium soft-magnetic alloy powder afterwards;
In the described water-gas combined atomization process stage, wherein atomized water is added with surfactant solution,
It is specially 17 alkenyl amine ethyl imidazol(e) hyamine ODD, and in atomized water, surfactant addition is
The 5wt% of atomized water total amount.
3) step 2) gained powder through powder collecting pot collect after, through bipyramid be vacuum dried, air current classifying
After, bolting.
After testing, the apparent density of this ferrum silicochromium soft-magnetic alloy powder is 2.98g/cm3, tap density is
4.4g/cm3;Oxygen content is less than 1500ppm;Under 600MPa, ring-shaped inductors green density is
6.42g/cm3, inductance Ls is 29.56 μ H.
Embodiment 2
The present embodiment is the comparative example of embodiment 1, and the present embodiment is with the difference of embodiment 1,
Step 2 in the present embodiment) in atomized water in be added without surfactant solution, by with embodiment 1
The silicochromium soft-magnetic alloy powder that taps a blast furnace is prepared under conditions of identical.
After testing, apparent density 2.48g/cm of this ferrum silicochromium soft-magnetic alloy powder3, tap density is
3.9g/cm3, oxygen content is higher than 2000ppm;Under 600MPa, ring-shaped inductors green density is
6.08g/cm3, inductance Ls is 23.7 μ H.
Embodiment 3
This enforcement is with the difference of embodiment 1: prepare ferrum silicochromium soft-magnetic alloy powder mistake in the present embodiment
In journey, surfactant addition is different, and in the present embodiment, the addition of this surfactant agent is atomization
The 2wt% of water inventory.
After testing, apparent density 2.92g/cm of this ferrum silicochromium soft-magnetic alloy powder3, tap density is
4.2g/cm3, oxygen content is less than 1500ppm;Under 600MPa, ring-shaped inductors green density is
6.33g/cm3, inductance Ls is 28.7 μ H.
Embodiment 4
The present embodiment is with the difference of embodiment 1, and in the atomized water of the present embodiment, surfactant adds
Amount is the 10wt% of atomized water total amount.
After testing, apparent density 2.67g/cm of this ferrum silicochromium soft-magnetic alloy powder3, tap density is
4.1g/cm3, oxygen content is less than 1800ppm;Under 600MPa, ring-shaped inductors green density is
6.27g/cm3, inductance Ls is 26.9 μ H.
Embodiment 5
The present embodiment is with the difference of embodiment 1, and in the atomized water of the present embodiment, surfactant adds
Kind is different, and in the present embodiment, surfactant selects sodium lauryl sulphate SDS, and surfactant adds
Enter the 5wt% that amount is atomized water total amount.
After testing, apparent density 2.66g/cm of this ferrum silicochromium soft-magnetic alloy powder3, tap density is
4.1g/cm3, oxygen content is less than 1500ppm;Under 600MPa, ring-shaped inductors green density is
6.12g/cm3, inductance Ls is 24.6 μ H.
Embodiment 6
The present embodiment is with the difference of embodiment 1, and in the atomized water of the present embodiment, surfactant adds
Kind is different, and in the present embodiment, surfactant selects Polyethylene Glycol PEG-600, and surfactant adds
Amount is the 10wt% of atomized water total amount.
After testing, apparent density 2.68g/cm of this ferrum silicochromium soft-magnetic alloy powder3, tap density is
4.1g/cm3, oxygen content is less than 1500ppm;Under 600MPa, ring-shaped inductors green density is
6.19g/cm3, inductance Ls is 25.9 μ H.
Another object of the present invention is to provide a kind of ferrum silicochromium soft magnetic powder, this ferrum silicochromium soft magnetic powder
Being prepared by preparation method recited above, can prepare high apparent density, high-tap density, hypoxia contains
The ferrum silicochromium powder that amount, inductance value and pcrmeability are higher.
It is still another object of the present invention to provide the application of a kind of ferrum silicochromium soft magnetic powder, this ferrum silicochromium is soft
Magnetic powder is prepared by preparation method recited above, using this ferrum silicochromium soft magnetic powder as miniature inductance
Raw material, such as such as chip inductor, ring-shaped inductors etc..
The foregoing is only the preferred embodiments of the present invention, all done with scope of the invention as claimed
Impartial change and modification, all should belong to the scope of the claims in the present invention.
Claims (10)
1. the preparation method of a ferrum silicochromium soft magnetic powder, it is characterised in that step is as follows:
1) adding in intermediate frequency furnace by ferrum silicochromium soft-magnetic alloy powder powder stock, air is smelted and is obtained alloy
Liquid;
2) under conditions of nitrogen is protected, aluminium alloy is sent into atomisation tower, during sending into, pass through
Supertension atomized water and lower scroll gas both atomizing mediums simultaneously act on aluminium alloy, by alloy
Liquid strength is broken into a large amount of fine metal molten drop, and cooled and solidified is ferrum silicochromium soft-magnetic alloy powder then.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 1, it is characterised in that
Described ferrum silicochromium soft-magnetic alloy powder raw materials quality ratio is: pure chromium 3.5-6.5%, pure silicon 3.0-6.5%,
Silicon calcium powder 0.6-0.8%, calcium oxide 1.0-1.5%, surplus is ferrum.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 2, it is characterised in that
Described 1), in the smelting process of step, control to smelt power 80-240KW;By pure chromium, pure silicon and ferrum
It is divided into two parts, during smelting, adds a pure chromium, pure silicon and ferrum prior to furnace bottom, change clear process and add successively
Enter another part of pure chromium, pure silicon and residue ferrum, and add before changing clearly;Control molten steel temperature >=1580-1600
DEG C, reducing power and to 10-30KW and add silicon calcium powder and calcium oxide covering molten steel, slag making removes the gred, pure
Change and obtain aluminium alloy.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 1, it is characterised in that
Described 2), in step, aluminium alloy is sent into atomisation tower and is first preliminarily formed bigger metal drop, afterwards by super
High-pressure atomization water and lower scroll gas both atomizing mediums act on described in bigger metal drop, will
This bigger metal drop strength is broken into a large amount of fine metal molten drop, and cooled and solidified is that ferrum silicochromium is soft then
Magnetic alloy powder.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 1, it is characterised in that
Described 2), in step, live in the surface adding the 1-15wt% accounting for atomized water gross weight in supertension atomized water
Property agent.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 5, it is characterised in that
Described surfactant is 17 alkenyl amine ethyl imidazol(e) hyamines, Polyethylene Glycol or dodecyl
Sodium sulfate.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 1, it is characterised in that
The pressure of described supertension atomized water is 120-150MPa.
The preparation method of a kind of ferrum silicochromium soft magnetic powder the most as claimed in claim 1, it is characterised in that
The pressure of described lower scroll gas is 0.2-0.6Mpa.
9. a ferrum silicochromium soft magnetic powder, it is characterised in that this ferrum silicochromium soft magnetic powder is wanted by right
The preparation method described in 1-8 is asked to prepare.
10. the application of a ferrum silicochromium soft magnetic powder, it is characterised in that this ferrum silicochromium soft magnetic powder leads to
Cross the preparation method described in claim 1-8 to prepare, using this ferrum silicochromium soft magnetic powder as miniature inductance
Raw material.
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