CN104078182A - Iron-based soft magnetic composite magnetic powder core and preparation method thereof - Google Patents
Iron-based soft magnetic composite magnetic powder core and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an iron-based soft magnetic composite magnetic powder core and a preparation method thereof. The invention adopts the technical scheme as follows: sequentially adding iron-based alloy powder, absolute ethyl alcohol, a silane coupling agent and distilled water into a reaction vessel according to the mass ratio of 1:(6-10):(0.04-0.10):(0.2-0.4), and stirring; adding tetraethyl orthosilicate or methyl silicate, then adding ammonia water, stirring continuously, washing, filtering and drying; placing the obtained composite powder with a core-shell heterostructure into an annealing furnace, performing heat preservation for 1-3 h under the condition of 600-800 DEG C, performing furnace cooling and performing compression moulding; sintering for 1-10 h under the condition of 900-1350 DEG C, so that the iron-based soft magnetic composite magnetic powder core is obtained after furnace cooling. The prepared iron-based soft magnetic composite magnetic powder core has the characteristics that the insulating property is good, the iron loss is low, high magnetic strength is achieved, the heat stability is good and the service life is prolonged when the iron-based soft magnetic composite magnetic powder core is used at a higher environment temperature.
Description
Technical field
The invention belongs to soft magnetism composite magnetic powder core technical field.Be specifically related to a kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.
Background technology
Powder core is the composite magnetic that a kind of soft magnetic powder is prepared by powder metallurgy process after insulating wrapped.Material according to forming powder core, can be divided into powder core ferrocart core, permalloy powder core, Fe-Si-Al magnetic core, amorphous powder core and nanocrystalline magnetic core etc.Iron-based powder core is a kind of magnetic material with high performance-price ratio, in fields such as circuit of power factor correction, pulse kickback transformer, energy storage filter inductor and line filters, has wide application space.But the raising of the operating frequency while applying with it, the iron loss of iron-based powder core can significantly raise, and especially eddy current loss increasing degree is larger.So the high-frequency vortex loss that how to reduce powder core is focus and the difficult point of current research.
In general, the major measure that reduces powder core eddy current loss is that Magnaglo is mixed with insulating compound, by insulating wrapped agent, Magnaglo is isolated, and the conductive path between blocking-up Magnaglo, improves the resistivity of powder core, thereby reduces eddy current loss.Wherein insulating wrapped agent used comprises the agent of organic resinae insulating wrapped and inorganic insulation covering.Due to organic resin class insulating compound non-refractory, powder core can only be heat-treated at a lower temperature.On the one hand, lower heat treatment temperature cause the relative density of powder core lower, intensity difference, steadiness be difficult to guarantee and saturated magnetic strength lower; On the other hand, powder core causes the easy ageing failure of organic resin because of eddy current loss heating at work, and powder core is destroyed." manufacture method of soft magnet silicon aluminium alloy powder core " be patented technology (CN1516204A), with epoxylite, be insulating compound, after moulding, under 600～800 ℃ of conditions, heat-treat, but because temperature is high, organic insulation agent has been decomposed and carbonization substantially, is difficult to the effect of performance insulation.
In recent years, inorganic insulation covering is because its excellent insulating properties and thermal stability become the focus of people's research gradually.The normal inorganic insulation covering using comprises mica, kaolin, talcum powder, Ludox and inorganic oxide etc.Preparation technology mixes ferromagnetic powder, insulating compound and binding agent, and die forming, obtains powder core after heat treatment.But prepared powder core has, insulating properties is poor, iron loss is larger, saturated magnetic strength is low and the defect of poor heat stability.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, and object has been to provide that a kind of insulation property are good, iron loss is low, high magnetic strength, Heat stability is good and compared with iron-based soft magnetic composite magnetic powder core of the long service life under high ambient temperature and preparation method thereof.
For achieving the above object, the concrete steps of the technical solution used in the present invention are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (6～10) ︰ (0.04～0.10) ︰ (0.2～0.4), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40～70 ℃ of conditions, stir 1～3h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 40～70 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add tetraethoxysilane or methyl silicate, then add ammoniacal liquor, continue to stir 8～24h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ tetraethoxysilane is 1 ︰ (0.2～2.0), the mass ratio of ferrous alloy powder ︰ methyl silicate is 1 ︰ (0.2～2.0); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.02～0.40).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 600～800 ℃ of conditions, is incubated 1～3h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 1～10h under 900～1350 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
Described iron(-)base powder is a kind of in pure iron, ferro-silicium and sendust; Fe content in described pure iron is greater than 99wt%; The Si content of described ferro-silicium is 0.1～10wt%; The Si content of described sendust is 4～13wt%, and Al content is 4～7wt%.
Described annealing furnace is the annealing furnace of vacuum protection or is the annealing furnace of inert gas shielding.
Described sintering furnace is the sintering furnace of vacuum protection or is the sintering furnace of inert gas shielding.
Described compressing pressure is 100～600MPa.
Employing is with technique scheme, and the present invention compared with prior art has the following advantages:
1. the present invention adopts chemical coating method, utilize the hydrolysis of tetraethoxysilane at iron(-)base powder surface coated silica insulating barrier, can guarantee the uniformity of each iron(-)base powder particle surface coated insulation layer, and can make silicon dioxide insulating layer thickness controllable.
2. prepared by the present invention, and to take the dispersiveness of the iron(-)base powder particle of iron(-)base powder in the iron-based soft magnetic composite magnetic powder core with nucleocapsid heterostructure that core, silicon dioxide insulating layer are shell better, between iron(-)base powder particle, by silicon dioxide insulating layer, isolated good insulating between iron(-)base powder particle.Eddy current is limited in insulating wrapped district, can effectively reduce the eddy current loss of iron-based soft magnetic composite magnetic powder core.
3. the iron-based soft magnetic composite magnetic powder core that prepared by the present invention does not adopt organic binder bond and organic insulation agent, the insulating compound silicon dioxide adopting can bear higher heat treatment temperature, iron-based soft magnetic composite magnetic powder core powder compact can carry out high-temperature heat treatment, the relative density of iron-based soft magnetic composite magnetic powder core improves obviously, the content of the ferromagnetic substance of unit volume also obviously improves, saturated magnetic strength is higher, and Heat stability is good can improve in the useful life compared with under high ambient temperature.
Iron-based soft magnetic composite magnetic powder core prepared by the present invention is after testing: magnetic permeability: μ (f=100KHz, 0.3V) is 123.4～147.8; Powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 76.9～83.5mW/cm
3; DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 40.4～44.0Oe.
Therefore, the present invention can effectively control thickness and the uniformity of iron-based soft magnetic composite magnetic powder in-core insulating coating, and prepared iron-based soft magnetic composite magnetic powder core has that insulation property are good, iron loss is low, high magnetic strength, Heat stability is good and in the feature of the long service life compared with under high ambient temperature.
Accompanying drawing explanation
Fig. 1 is the cross section stereoscan photograph of a kind of iron-based soft magnetic composite magnetic powder core of preparing of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described, not the restriction to its protection range.
For avoiding repetition, now iron(-)base powder unification described in this embodiment is described below, in embodiment, repeat no more:
Fe content in described pure iron is greater than 99wt%;
The Si content of described ferro-silicium is 0.1～10.0wt%;
The Si content of described sendust is 4～13wt%, and Al content is 4～7wt%.
Embodiment 1
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By iron(-)base powder Fen Mo ︰, Wu the mass ratio of Shui Yi Chun ︰ Gui alkane Ou Lian Ji ︰ distilled water, be 1 ︰ (6～7) ︰ (0.04～0.05) ︰ (0.20～0.25), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40～45 ℃ of conditions, stir 1.5～2.0h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 40～45 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add tetraethoxysilane, then add ammoniacal liquor, continue to stir 8～10h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ tetraethoxysilane is 1 ︰ (0.2～0.4); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.02～0.05).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 600～650 ℃ of conditions, is incubated 1.5～2.0h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 2～4h under 900～1000 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is pure iron powder; Compressing pressure is 100～200MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 147.2～147.8;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 82.4～83.5mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 43.2～43.5Oe.
Embodiment 2
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (7～8) ︰ (0.05～0.06) ︰ (0.25～0.30), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 45～50 ℃ of conditions, stir 2.5～3.0h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 45～50 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add methyl silicate, then add ammoniacal liquor, continue to stir 10～12h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ methyl silicate is 1 ︰ (0.4～0.6); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.05～0.10).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 650～700 ℃ of conditions, is incubated 2.0～2.5h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 4～6h under 1000～1050 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is ferro-silicium powder; Compressing pressure is 200～300MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 124.0～139.4;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 79.4～83.0mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 42.2～44.0Oe.
Embodiment 3
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (8～9) ︰ (0.06～0.07) ︰ (0.30～0.35), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 50～55 ℃ of conditions, stir 1.0～1.5h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 50～55 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add tetraethoxysilane, then add ammoniacal liquor, continue to stir 12～14h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ tetraethoxysilane is 1 ︰ (0.6～1.0); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.10～0.15).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 700～750 ℃ of conditions, is incubated 2.5～3.0h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 6～8h under 1050～1100 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is sendust powder; Compressing pressure is 300～400MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 124.7～127.3;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 80.5～81.1mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 42.0～42.7Oe.
Embodiment 4
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (9～10) ︰ (0.07～0.08) ︰ (0.35～0.40), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 55～60 ℃ of conditions, stir 2.0～2.5h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 55～60 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add methyl silicate, then add ammoniacal liquor, continue to stir 14～16h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ methyl silicate is 1 ︰ (1.0～1.2); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.15～0.20).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 750～800 ℃ of conditions, is incubated 1.0～1.5h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 8～10h under 1100～1150 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is pure iron powder; Compressing pressure is 400～500MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 146.2～147.4;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 81.6～82.4mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 42.9～43.4Oe.
Embodiment 5
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (6.0～6.5) ︰ (0.08～0.09) ︰ (0.2～0.3), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 60～65 ℃ of conditions, stir 1.5～2.0h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 60～65 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add tetraethoxysilane, then add ammoniacal liquor, continue to stir 16～18h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ tetraethoxysilane is 1 ︰ (1.2～1.4); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.20～0.25).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 600～700 ℃ of conditions, is incubated 1～2h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 1～3h under 1150～1200 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is ferro-silicium powder; Compressing pressure is 500～600MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 123.5～135.1;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 78.3～82.6mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 41.0～43.5Oe.
Embodiment 6
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (6.5～8.0) ︰ (0.09～0.10) ︰ (0.3～0.4), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 65～70 ℃ of conditions, stir 2.5～3.0h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 65～70 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add methyl silicate, then add ammoniacal liquor, continue to stir 18～20h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ methyl silicate is 1 ︰ (1.4～1.6); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.25～0.30).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 700～800 ℃ of conditions, is incubated 2～3h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 3～5h under 1200～1250 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is sendust powder; Compressing pressure is 350～400MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 124.1～126.9;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 80.6～81.0mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 41.7～42.4Oe.
Embodiment 7
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (8.0～8.5) ︰ (0.04～0.07) ︰ (0.25～0.35), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40～55 ℃ of conditions, stir 1～2h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 40～55 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add tetraethoxysilane, then add ammoniacal liquor, continue to stir 20～22h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ tetraethoxysilane is 1 ︰ (1.6～1.8); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.30～0.35).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 730～780 ℃ of conditions, is incubated 1.0～1.5h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 5～7h under 1250～1300 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is ferro-silicium powder; Compressing pressure is 400～450MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 123.4～136.7;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 76.9～81.3mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 40.4～43.0Oe.
Embodiment 8
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Described in the present embodiment, preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (8.5～10.0) ︰ (0.07～0.10) ︰ (0.30～0.35), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 55～70 ℃ of conditions, stir 2～3h, obtain the mixed solution containing the iron(-)base powder of surface modification.
The preparation of second step, nucleocapsid heterostructure composite powder
Under 55～70 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add methyl silicate, then add ammoniacal liquor, continue to stir 22～24h; Then use absolute ethanol washing 3～5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder.
Wherein: the mass ratio of ferrous alloy powder ︰ methyl silicate is 1 ︰ (1.8～2.0); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.35～0.40).
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 780～800 ℃ of conditions, is incubated 1.5～2.0h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing.
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact.
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 7～10h under 1300～1350 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
In the present embodiment: iron(-)base powder is sendust powder; Compressing pressure is 450～500MPa.
Iron-based soft magnetic composite magnetic powder core prepared by the present embodiment is after testing:
(1) magnetic permeability: μ (f=100KHz, 0.3V) is 123.8～125.0;
(2) powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 79.8～81.1mW/cm
3;
(3) DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 40.8～41.4Oe.
This embodiment compared with prior art has the following advantages:
1. this embodiment adopts chemical coating method, utilize the hydrolysis of tetraethoxysilane at iron(-)base powder surface coated silica insulating barrier, can guarantee the uniformity of each iron(-)base powder particle surface coated insulation layer, and can make silicon dioxide insulating layer thickness controllable.
2. prepared by this embodiment, and to take the dispersiveness of the iron(-)base powder particle of iron(-)base powder in the iron-based soft magnetic composite magnetic powder core with nucleocapsid heterostructure that core, silicon dioxide insulating layer are shell better, between iron(-)base powder particle, by silicon dioxide insulating layer, isolated, good insulating between iron(-)base powder particle, be illustrated in figure 1 the cross section stereoscan photograph of embodiment 1 prepared sample, the iron(-)base powder particle in powder core is by SiO
2evenly coated, realized the intergranular insulation of ferrous alloy.Eddy current is limited in insulating wrapped district, can effectively reduce the eddy current loss of iron-based soft magnetic composite magnetic powder core.
3. the iron-based soft magnetic composite magnetic powder core that prepared by this embodiment does not adopt organic binder bond and organic insulation agent, the insulating compound silicon dioxide adopting can bear higher heat treatment temperature, iron-based soft magnetic composite magnetic powder core powder compact can carry out high-temperature heat treatment, the relative density of iron-based soft magnetic composite magnetic powder core improves obviously, the content of the ferromagnetic substance of unit volume also obviously improves, saturated magnetic strength is higher, and Heat stability is good can improve in the useful life compared with under high ambient temperature.
Iron-based soft magnetic composite magnetic powder core prepared by this embodiment is after testing: magnetic permeability: μ (f=100KHz, 0.3V) is 123.4～147.8; Powder core volume ratio loss: 50KHz, during 500Gs, P
cvbe 76.9～83.5mW/cm
3; DC stacked: under 100KHz, when magnetic permeability drops to 50%, direct current biasing field is that H is 40.4～44.0Oe.
Therefore, this embodiment can effectively be controlled thickness and the uniformity of iron-based soft magnetic composite magnetic powder in-core insulating coating, and prepared iron-based soft magnetic composite magnetic powder core has that insulation property are good, iron loss is low, high magnetic strength, Heat stability is good and in the feature of the long service life compared with under high ambient temperature.
Claims (6)
1. a preparation method for iron-based soft magnetic composite magnetic powder core, is characterized in that described preparation method's concrete steps are:
The surface modification of the first step, iron(-)base powder
By ferrous alloy powder ︰, without the even mass ratio that joins agent ︰ distilled water of water second alcohol ︰ silicon alkane, be 1 ︰ (6 ~ 10) ︰ (0.04 ~ 0.10) ︰ (0.2 ~ 0.4), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are added in reaction vessel successively, under 40 ~ 70 ℃ of conditions, stir 1 ~ 3h, obtain the mixed solution containing the iron(-)base powder of surface modification;
The preparation of second step, nucleocapsid heterostructure composite powder
Under 40 ~ 70 ℃ and stirring condition, first in the mixed solution of the described iron(-)base powder containing surface modification, add tetraethoxysilane or methyl silicate, then add ammoniacal liquor, continue to stir 8 ~ 24h; Then use absolute ethanol washing 3 ~ 5 times, filter, vacuumize, obtains nucleocapsid heterostructure composite powder;
Wherein: the mass ratio of ferrous alloy powder ︰ tetraethoxysilane is 1 ︰ (0.2 ~ 2.0), the mass ratio of ferrous alloy powder ︰ methyl silicate is 1 ︰ (0.2 ~ 2.0); The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.02 ~ 0.40);
The 3rd step, annealing heat treatment
The nucleocapsid heterostructure composite powder that second step is obtained is inserted in annealing furnace, under 600 ~ 800 ℃ of conditions, is incubated 1 ~ 3h, cools to room temperature with the furnace, obtains the heat treated nucleocapsid heterostructure composite powder of annealing;
The preparation of the 4th step, powder compact
The nucleocapsid heterostructure composite powder that the annealing in process that the 3rd step is obtained is crossed is compressing, obtains iron-based soft magnetic composite magnetic powder core powder compact;
The preparation of the 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that the 4th step is obtained is inserted in sintering furnace, and sintering 1 ~ 10h under 900 ~ 1350 ℃ of conditions, cools to room temperature with the furnace, obtains iron-based soft magnetic composite magnetic powder core.
2. the preparation method of iron-based soft magnetic composite magnetic powder core according to claim 1, is characterized in that described iron(-)base powder is a kind of in pure iron, ferro-silicium and sendust; Fe content in described pure iron is greater than 99wt%; The Si content of described ferro-silicium is 0.1 ~ 10.0wt%; The Si content of described sendust is 4 ~ 13wt%, and Al content is 4 ~ 7wt%.
3. the preparation method of iron-based soft magnetic composite magnetic powder core according to claim 1, is characterized in that described annealing furnace is the annealing furnace of vacuum protection or is the annealing furnace of inert gas shielding.
4. the preparation method of iron-based soft magnetic composite magnetic powder core according to claim 1, is characterized in that described sintering furnace is the sintering furnace of vacuum protection or is the sintering furnace of inert gas shielding.
5. according to the preparation method of the composite magnetic powder core of iron-based soft magnetic described in claim 1, it is characterized in that described compressing pressure is 100 ~ 600MPa.
6. an iron-based soft magnetic composite magnetic powder core, is characterized in that described iron-based soft magnetic composite magnetic powder core is according to the prepared iron-based soft magnetic composite magnetic powder core of preparation method of the iron-based soft magnetic composite magnetic powder core described in any one in claim 1 ~ 5.
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