CN104078182B - A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof - Google Patents
A kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof Download PDFInfo
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- CN104078182B CN104078182B CN201410355695.5A CN201410355695A CN104078182B CN 104078182 B CN104078182 B CN 104078182B CN 201410355695 A CN201410355695 A CN 201410355695A CN 104078182 B CN104078182 B CN 104078182B
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Abstract
The present invention relates to a kind of iron-based soft magnetic composite magnetic powder core and preparation method thereof.Its technical scheme is：The mass ratio for occasionally joining agent ︰ distilled water without water second alcohol ︰ silicon alkane by ferrous alloy powder ︰ sequentially adds iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water in reaction vessel for 1 ︰ (6 ~ 10) ︰ (0.04 ~ 0.10) ︰ (0.2 ~ 0.4), stirs；Tetraethyl orthosilicate or methyl silicate are added thereto, ammoniacal liquor is added, continues to stir, is washed, is filtered, and are dried；Then obtained nucleocapsid heterojunction structure composite powder is inserted in annealing furnace, 1 ~ 3h is incubated under the conditions of 600 ~ 800 DEG C, furnace cooling is compressing；1 ~ 10h is finally sintered under the conditions of 900 ~ 1350 DEG C, furnace cooling, produces iron-based soft magnetic composite magnetic powder core.Iron-based soft magnetic composite magnetic powder core prepared by the present invention has the characteristics of insulating properties are good, iron loss is low, high magnetic strength, heat endurance are good and can improve service life at higher ambient temperatures.
Description
Technical field
The invention belongs to soft magnetism composite magnetic powder core technical field.More particularly to a kind of iron-based soft magnetic composite magnetic powder core and its system
Preparation Method.
Background technology
Powder core is the composite magnetic that a kind of soft magnetic powder is prepared after insulating wrapped by powder metallurgy process.Root
According to the material for forming powder core, powder core can be divided into ferrocart core, permalloy powder core, Fe-Si-Al magnetic core, amorphous magnetic
Core and nanocrystalline magnetic core etc..Iron-based powder core is a kind of magnetic material with high performance-price ratio, circuit of power factor correction,
The fields such as pulse kickback transformer, energy storage filter inductor and line filter have wide application space.But with its application
When working frequency raising, the iron loss of iron-based powder core can raise significantly, and especially eddy-current loss increasing degree is larger.Institute
How to reduce focus and difficult point that the high frequency eddy current losses of powder core are current researches.
In general, the major measure for reducing powder core eddy-current loss is to mix Magnaglo with insulating compound, by exhausted
Edge covering isolates Magnaglo, blocks the conductive path between Magnaglo, the resistivity of powder core is improved, so as to reduce
Eddy-current loss.Insulating wrapped agent wherein used includes organic resinae insulating wrapped agent and inorganic insulation covering.Due to having
Machine resinae insulating compound non-refractory, powder core can only be heat-treated at a lower temperature.On the one hand, relatively low heat treatment temperature
Degree causes that the relatively low relative density of powder core, intensity difference, steadiness are difficult to ensure that and saturation magnetic strength is relatively low；On the other hand, magnetic
Core causes the easy ageing failure of organic resin because of eddy-current loss heating at work, destroys powder core." soft magnet silicon aluminium alloy
The manufacture method of powder core " (CN1516204A) patented technology, using epoxylite as insulating compound, in 600~800 DEG C of bars after shaping
It is heat-treated under part, but because temperature is high, organic insulation agent has been decomposed and has been carbonized substantially, it is difficult to plays the effect of insulation.
In recent years, inorganic insulation covering is increasingly becoming the heat of people's research due to its excellent insulating properties and heat endurance
Point.The inorganic insulation covering often used includes mica, kaolin, talcum powder, Ludox and inorganic oxide etc..Preparation technology
It is to mix ferromagnetic powder, insulating compound and binding agent, die forming, powder core is obtained after heat treatment.But prepared powder core
It there are the defects of insulating properties is poor, iron loss is larger, saturation magnetic strength is low and heat endurance is poor.
The content of the invention
It is contemplated that overcome the deficiencies in the prior art, it is therefore an objective to provide that a kind of insulating properties are good, iron loss is low, Gao Ci
Sense, heat endurance be good and iron-based soft magnetic composite magnetic powder core and preparation method thereof for being grown compared with the service life under high environment temperature.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
By ferrous alloy powder ︰ without water second alcohol ︰ silicon alkane occasionally connection agent ︰ distilled water mass ratio for 1 ︰ (6~10) ︰ (0.04~
0.10) ︰ (0.2~0.4), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are sequentially added into reaction vessel
It is interior, 1~3h is stirred under the conditions of 40~70 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 40~70 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Tetraethyl orthosilicate or methyl silicate are added, ammoniacal liquor is added, continues 8~24h of stirring；Then 3~5 are washed with absolute ethyl alcohol
It is secondary, filter, vacuum drying, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ tetraethyl orthosilicates is 1 ︰ (0.2~2.0), the positive silicon of ferrous alloy powder ︰
The mass ratio of sour methyl esters is 1 ︰ (0.2~2.0)；The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.02~0.40).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 600~800 DEG C
1~3h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 900~1350 DEG C of bars
1~10h is sintered under part, room temperature is cooled to the furnace, produces iron-based soft magnetic composite magnetic powder core.
The iron(-)base powder is one kind in pure iron, ferro-silicium and sendust；Fe in the pure iron contains
Amount is more than 99wt%；The Si contents of the ferro-silicium are 0.1~10wt%；The Si contents of the sendust be 4~
13wt%, Al content are 4~7wt%.
The annealing furnace be the annealing furnace of vacuum protection or be inert gas shielding annealing furnace.
The sintering furnace be the sintering furnace of vacuum protection or be inert gas shielding sintering furnace.
The compressing pressure is 100~600MPa.
Using techniques described above scheme, the present invention has advantages below compared with prior art：
1. the present invention uses chemical coating method, wrapped using the hydrolysis of tetraethyl orthosilicate on iron(-)base powder surface
Silicon dioxide insulating layer is covered, can guarantee that the uniformity of each iron(-)base powder particle surface coated insulation layer, and dioxy can be made
SiClx thickness of insulating layer is controllable.
2. prepared by the present invention has nucleocapsid heterojunction structure using iron(-)base powder as core, silicon dioxide insulating layer for shell
Iron-based soft magnetic composite magnetic powder core in iron(-)base powder particle dispersiveness preferably, by dioxy between iron(-)base powder particle
SiClx insulator separation, good insulating between iron(-)base powder particle.Vortex is limited in insulating wrapped area, can effectively reduce
The eddy-current loss of iron-based soft magnetic composite magnetic powder core.
3. iron-based soft magnetic composite magnetic powder core prepared by the present invention does not use organic binder bond and organic insulation agent, used
Insulating compound silica can bear higher heat treatment temperature, and iron-based soft magnetic composite magnetic powder core powder compact can be carried out at high warm
Reason, the relative density of iron-based soft magnetic composite magnetic powder core are obviously improved, and the content of the ferromagnetic material of unit volume also significantly improves,
Saturation magnetic strength is higher, and heat endurance is good, can improve service life at higher ambient temperatures.
Iron-based soft magnetic composite magnetic powder core prepared by the present invention is after testing：Magnetic conductivity：μ (f=100KHz, 0.3V) is 123.4
~147.8；Powder core volume specific loss：When 50KHz, 500Gs, PcvFor 76.9~83.5mW/cm3；It is DC stacked：100KHz
Under, when magnetic conductivity drops to 50%, direct current biasing field is that H is 40.4~44.0Oe.
Therefore, the present invention can effectively control the thickness and uniformity of iron-based soft magnetic composite magnetic powder core interior insulation clad, institute
The iron-based soft magnetic composite magnetic powder core of preparation has that insulating properties are good, iron loss is low, high magnetic strength, heat endurance are good and in higher environment
At a temperature of service life it is long the characteristics of.
Brief description of the drawings
Fig. 1 is a kind of cross-sectional scans electromicroscopic photograph of iron-based soft magnetic composite magnetic powder core prepared by the present invention.
Embodiment
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
It is now that iron(-)base powder Unify legislation described in present embodiment is as follows to avoid repeating, in embodiment not
Repeat again：
Fe contents in the pure iron are more than 99wt%；
The Si contents of the ferro-silicium are 0.1~10.0wt%；
The Si contents of the sendust are 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
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 sequentially added into reaction and held
In device, 1.5~2.0h is stirred under the conditions of 40~45 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 40~45 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Tetraethyl orthosilicate is added, ammoniacal liquor is added, continues 8~10h of stirring；Then washed 3~5 times, filtered with absolute ethyl alcohol, vacuum is done
It is dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ tetraethyl orthosilicates is 1 ︰ (0.2~0.4)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.02~0.05).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 600~650 DEG C
1.5~2.0h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 900~1000 DEG C of bars
2~4h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 147.2~147.8；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 82.4~83.5mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
By ferrous alloy powder ︰ without water second alcohol ︰ silicon alkane occasionally connection agent ︰ distilled water mass ratio for 1 ︰ (7~8) ︰ (0.05~
0.06) ︰ (0.25~0.30), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are sequentially added into reaction vessel
It is interior, 2.5~3.0h is stirred under the conditions of 45~50 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 45~50 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Methyl silicate is added, ammoniacal liquor is added, continues 10~12h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ methyl silicates is 1 ︰ (0.4~0.6)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.05~0.10).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 650~700 DEG C
2.0~2.5h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1000~1050 DEG C of bars
4~6h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 124.0~139.4；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 79.4~83.0mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
By ferrous alloy powder ︰ without water second alcohol ︰ silicon alkane occasionally connection agent ︰ distilled water mass ratio for 1 ︰ (8~9) ︰ (0.06~
0.07) ︰ (0.30~0.35), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are sequentially added into reaction vessel
It is interior, 1.0~1.5h is stirred under the conditions of 50~55 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 50~55 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Tetraethyl orthosilicate is added, ammoniacal liquor is added, continues 12~14h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ tetraethyl orthosilicates is 1 ︰ (0.6~1.0)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.10~0.15).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 700~750 DEG C
2.5~3.0h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1050~1100 DEG C of bars
6~8h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 124.7~127.3；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 80.5~81.1mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
By ferrous alloy powder ︰ without water second alcohol ︰ silicon alkane occasionally connection agent ︰ distilled water mass ratio for 1 ︰ (9~10) ︰ (0.07~
0.08) ︰ (0.35~0.40), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are sequentially added into reaction vessel
It is interior, 2.0~2.5h is stirred under the conditions of 55~60 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 55~60 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Methyl silicate is added, ammoniacal liquor is added, continues 14~16h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ methyl silicates is 1 ︰ (1.0~1.2)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.15~0.20).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 750~800 DEG C
1.0~1.5h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1100~1150 DEG C of bars
8~10h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 146.2~147.4；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 81.6~82.4mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
The mass ratio for occasionally joining agent ︰ distilled water without water second alcohol ︰ silicon alkane by ferrous alloy powder ︰ is 1 ︰ (6.0~6.5) ︰ (0.08
~0.09) ︰ (0.2~0.3), reaction vessel is sequentially added by iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water
It is interior, 1.5~2.0h is stirred under the conditions of 60~65 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 60~65 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Tetraethyl orthosilicate is added, ammoniacal liquor is added, continues 16~18h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ tetraethyl orthosilicates is 1 ︰ (1.2~1.4)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.20~0.25).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 600~700 DEG C
1~2h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1150~1200 DEG C of bars
1~3h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 123.5~135.1；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 78.3~82.6mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
The mass ratio for occasionally joining agent ︰ distilled water without water second alcohol ︰ silicon alkane by ferrous alloy powder ︰ is 1 ︰ (6.5~8.0) ︰ (0.09
~0.10) ︰ (0.3~0.4), reaction vessel is sequentially added by iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water
It is interior, 2.5~3.0h is stirred under the conditions of 65~70 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 65~70 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Methyl silicate is added, ammoniacal liquor is added, continues 18~20h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ methyl silicates is 1 ︰ (1.4~1.6)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.25~0.30).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 700~800 DEG C
2~3h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1200~1250 DEG C of bars
3~5h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 124.1~126.9；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 80.6~81.0mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
The mass ratio for occasionally joining agent ︰ distilled water without water second alcohol ︰ silicon alkane by ferrous alloy powder ︰ is 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 sequentially added into reaction and held
In device, 1~2h is stirred under the conditions of 40~55 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 40~55 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Tetraethyl orthosilicate is added, ammoniacal liquor is added, continues 20~22h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ tetraethyl orthosilicates is 1 ︰ (1.6~1.8)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.30~0.35).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 730~780 DEG C
1.0~1.5h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1250~1300 DEG C of bars
5~7h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 123.4~136.7；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 76.9~81.3mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity 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.Preparation method described in the present embodiment comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
The mass ratio for occasionally joining agent ︰ distilled water without water second alcohol ︰ silicon alkane by ferrous alloy powder ︰ is 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 sequentially added
In reaction vessel, 2~3h is stirred under the conditions of 55~70 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface.
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 55~70 DEG C and stirring condition, first into the mixed solution of the iron(-)base powder being modified containing surface
Methyl silicate is added, ammoniacal liquor is added, continues 22~24h of stirring；Then washed 3~5 times, filtered, vacuum with absolute ethyl alcohol
Dry, obtain nucleocapsid heterojunction structure composite powder.
Wherein：The mass ratio of ferrous alloy powder ︰ methyl silicates is 1 ︰ (1.8~2.0)；Ferrous alloy powder ︰ ammoniacal liquor
Mass ratio be 1 ︰ (0.35~0.40).
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, is incubated under the conditions of 780~800 DEG C
1.5~2.0h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed.
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains iron-based soft magnetic and answers
Close powder core powder compact.
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, in 1300~1350 DEG C of bars
7~10h is sintered under part, room temperature is cooled to the furnace, produces 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 manufactured in the present embodiment is after testing：
(1) magnetic conductivity：μ (f=100KHz, 0.3V) is 123.8~125.0；
(2) powder core volume specific loss：When 50KHz, 500Gs, PcvFor 79.8~81.1mW/cm3；
(3) it is DC stacked：Under 100KHz, when magnetic conductivity drops to 50%, direct current biasing field is that H is 40.8~41.4Oe.
Present embodiment has advantages below compared with prior art：
1. present embodiment uses chemical coating method, using the hydrolysis of tetraethyl orthosilicate in fe-based alloy powder
Last Surface coating silicon dioxide insulating layer, the uniformity of each iron(-)base powder particle surface coated insulation layer is can guarantee that, and
Silicon dioxide insulating layer thickness can be made controllable.
2. prepared by present embodiment has nucleocapsid using iron(-)base powder as core, silicon dioxide insulating layer for shell
The dispersiveness of iron(-)base powder particle in the iron-based soft magnetic composite magnetic powder core of heterojunction structure is preferable, iron(-)base powder particle
Between isolated by silicon dioxide insulating layer, good insulating between iron(-)base powder particle, as shown in Figure 1 is sample prepared by embodiment 1
The cross-sectional scans electromicroscopic photograph of product, the iron(-)base powder particle in powder core is by SiO2Uniformly cladding, realizes ferrous alloy
Intergranular insulation.Vortex is limited in insulating wrapped area, can effectively reduce the eddy-current loss of iron-based soft magnetic composite magnetic powder core.
3. iron-based soft magnetic composite magnetic powder core prepared by present embodiment does not use organic binder bond and organic insulation agent,
Used insulating compound silica can bear higher heat treatment temperature, and iron-based soft magnetic composite magnetic powder core powder compact can be carried out
High-temperature heat treatment, the relative density of iron-based soft magnetic composite magnetic powder core are obviously improved, and the content of the ferromagnetic material of unit volume is also
Significantly improve, saturation magnetic strength is higher, and heat endurance is good, can improve service life at higher ambient temperatures.
Iron-based soft magnetic composite magnetic powder core prepared by present embodiment is after testing：Magnetic conductivity：μ (f=100KHz, 0.3V)
For 123.4~147.8；Powder core volume specific loss：When 50KHz, 500Gs, PcvFor 76.9~83.5mW/cm3；It is DC stacked：
Under 100KHz, when magnetic conductivity drops to 50%, direct current biasing field is that H is 40.4~44.0Oe.
Therefore, present embodiment can effectively control iron-based soft magnetic composite magnetic powder core interior insulation clad thickness and
Even property, prepared iron-based soft magnetic composite magnetic powder core have that insulating properties are good, iron loss is low, high magnetic strength, heat endurance are good and
The characteristics of long compared with service life under high environment temperature.
Claims (4)
1. a kind of preparation method of iron-based soft magnetic composite magnetic powder core, it is characterised in that the preparation method comprises the concrete steps that：
The first step, the surface of iron(-)base powder are modified
By ferrous alloy powder ︰ without water second alcohol ︰ silicon alkane occasionally connection agent ︰ distilled water mass ratio for 1 ︰ (6~10) ︰ (0.04~
0.10) ︰ (0.2~0.4), iron(-)base powder, absolute ethyl alcohol, silane coupler and distilled water are sequentially added into reaction vessel
It is interior, 1~3h is stirred under the conditions of 40~70 DEG C, obtains the mixed solution of iron(-)base powder being modified containing surface；The iron-based
Alloy powder is sendust, and the Si contents of sendust are 4~13wt%, and Al content is 4~7wt%；
The preparation of second step, nucleocapsid heterojunction structure composite powder
Under 40~70 DEG C and stirring condition, first added into the mixed solution of the iron(-)base powder being modified containing surface
Tetraethyl orthosilicate or methyl silicate, add ammoniacal liquor, continue 8~24h of stirring；Then 3~5 times are washed with absolute ethyl alcohol, mistake
Filter, vacuum drying, obtains nucleocapsid heterojunction structure composite powder；
Wherein：The mass ratio of ferrous alloy powder ︰ tetraethyl orthosilicates is 1 ︰ (0.2~2.0), the positive silicic acid first of ferrous alloy powder ︰
The mass ratio of ester is 1 ︰ (0.2~2.0)；The mass ratio of ferrous alloy powder ︰ ammoniacal liquor is 1 ︰ (0.02~0.40)；
3rd step, annealing heat-treats
The nucleocapsid heterojunction structure composite powder that second step obtains is inserted in annealing furnace, under the conditions of 600~800 DEG C be incubated 1~
3h, cool to room temperature with the furnace, obtain the nucleocapsid heterojunction structure composite powder that annealing heat-treats are crossed；
The preparation of 4th step, powder compact
The nucleocapsid heterojunction structure composite powder made annealing treatment that 3rd step is obtained is compressing, obtains the compound magnetic of iron-based soft magnetic
Powder core powder compact；The compressing pressure is 100~600MPa；
The preparation of 5th step, iron-based soft magnetic composite magnetic powder core
The iron-based soft magnetic composite magnetic powder core powder compact that 4th step obtains is inserted in sintering furnace, under the conditions of 900~1350 DEG C
1~10h is sintered, room temperature is cooled to the furnace, produces 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, it is characterised in that the annealing furnace is true
The annealing furnace or the annealing furnace for inert gas shielding of sky protection.
3. the preparation method of iron-based soft magnetic composite magnetic powder core according to claim 1, it is characterised in that the sintering furnace is true
The sintering furnace or the sintering furnace for inert gas shielding of sky protection.
4. a kind of iron-based soft magnetic composite magnetic powder core, it is characterised in that the iron-based soft magnetic composite magnetic powder core is according to claim 1
Iron-based soft magnetic composite magnetic powder core prepared by the preparation method of iron-based soft magnetic composite magnetic powder core any one of~3.
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| JP6930722B2 (en) * | 2017-06-26 | 2021-09-01 | 太陽誘電株式会社 | Manufacturing method of magnetic material, electronic component and magnetic material |
| CN107492433B (en) * | 2017-07-05 | 2019-08-16 | 铜陵江威科技有限公司 | A kind of iron-based soft magnetic composite material and preparation method of doping vario-property nickel powder |
| CN107498035A (en) * | 2017-07-05 | 2017-12-22 | 安徽江威精密制造有限公司 | A kind of iron-based soft magnetic composite of corrosion-resistant high permeability and preparation method thereof |
| CN108597719A (en) * | 2018-06-07 | 2018-09-28 | 上海海事大学 | A kind of preparation method of FeSiAl bases soft-magnetic composite material |
| CN111112601B (en) * | 2018-11-01 | 2021-10-01 | 哈尔滨工业大学 | High-temperature-resistant ferromagnetic wave absorbing agent, preparation method thereof and application of high-temperature-resistant ferromagnetic wave absorbing agent in preparation of high-temperature-resistant ferromagnetic wave absorbing material |
| CN109786096B (en) * | 2018-12-14 | 2021-07-23 | 浙江工业大学 | Two-dimensional layered metal soft magnetic composite material and preparation method and application thereof |
| CN110246679B (en) * | 2019-07-31 | 2020-12-22 | 合肥工业大学 | Preparation method of metal soft magnetic powder core based on organic/inorganic composite insulation process |
| CN112086257B (en) * | 2019-10-24 | 2023-07-25 | 中国科学院宁波材料技术与工程研究所 | Magnetic powder core with high magnetic conductivity and high quality factor, and preparation method and application thereof |
| CN110767441B (en) * | 2019-11-06 | 2022-04-05 | 安徽工业大学 | FeSiBCr/SiO2Preparation method of nanocrystalline soft magnetic composite iron core |
| CN111192735A (en) * | 2020-01-17 | 2020-05-22 | 深圳市铂科新材料股份有限公司 | Insulation coated metal soft magnetic powder and preparation method and application thereof |
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