CN104078181A - Iron-based alloy magnetic powder core adopting core-shell heterostructure and preparation method thereof - Google Patents
Iron-based alloy magnetic powder core adopting core-shell heterostructure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an iron-based alloy magnetic powder core adopting a core-shell heterostructure and a preparation method thereof. The technical scheme is as follows: 80-95wt% of iron-based alloy powder and 5-20wt% of inorganic oxide powder are evenly mixed and subjected to ball milling for 1-5 h under the shielding of an inert gas, the ball-milled iron-based alloy composite powder is contained in a graphite die, then the graphite die is placed in a plasma activation sintering furnace to be heated to 900-1250 DEG C, the pressure is exerted on the graphite die to 20-50 MPa, and the temperature is kept for 5-30 min under the shielding of the inert gas; the temperature is reduced to 400-500 DEG C at the temperature reduction rate of 30-50 DEG C/min, and the graphite die is cooled along with the furnace; the pressure exerted on the graphite die is unchanged when the temperature is kept and reduced to 400-500 DEG C, and the pressure is reduced to 0 at a constant speed during cooling; the graphite die is taken out of the furnace, and demolding is performed to obtain the iron-based alloy magnetic powder core adopting the core-shell heterostructure. The preparation method is simple in process, high in preparation efficiency and low in preparation cost; the iron-based alloy magnetic powder core is high in saturation flux density, high in density, good in insulating property, low in eddy-current loss and good in thermal stability.
Description
Technical field
The invention belongs to ferrous alloy powder core technical field.Be specifically related to a kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.
Background technology
Powder core is by ferromagnetic powder particle, to be mixed a kind of soft magnetic material that compacting forms with dielectric, is called again soft-magnetic composite material or compressed-core.Because the surface at ferromagnetic powder particle is being coated one deck dielectric insulating film, the resistivity of powder core is high, thereby eddy current loss is low, is suitable for upper frequency application.In addition, powder core also has the advantages such as higher saturation induction density, good frequency characteristic and permanent magnetic conduction, make powder core as inductance filter, choking-winding, be widely used in the fields such as communication, the energy, auto industry, household appliances and auto-door controlling, become one of important part of soft magnetic material.
Powder core mainly contains ferromagnetic powder core, sendust powder core, iron-nickel alloy powder core, ferrum-silicon alloy magnetic powder core, permalloy powder core etc.The preparation method of ferrous alloy powder core is generally by after ferrous alloy Magnaglo and the mixing of resinae insulating compound at present, after compression molding and heat treatment, obtains.Ferrous alloy powder core prepared by this method, under higher temperature conditions, during heat treatment, can there is thermal decomposition and carbonization in the resin that is coated on magnetic surface, causes that insulating properties declines, high-gradient magnetism can be not good, eddy current loss is larger.In addition, the another one unfavorable factor that adopts organic insulation agent is that powder core generates heat and makes organic substance aging because of long-term eddy current loss at work, thereby affects the stability of powder core performance." manufacture method of soft magnet silicon aluminium alloy powder core " (CN1516204A) patented technology adopts epoxies insulating compound, a kind of as in 607 epoxy resin, 609 epoxy resin, W-6A magnetic binding agent, W-6C magnetic binding agent, the dilution of binding agent is organic solvent absolute ethyl alcohol, acetone, ethyl acetate.After moulding, at 600 ~ 800 ℃, heat-treat.But under said temperature, organic insulation agent has been decomposed and carbonization substantially.
In recent years, inorganic insulation is coated because its excellent insulating properties and thermal stability become the focus of people's research gradually.The normal inorganic insulation agent of using comprises inorganic phosphate (zinc phosphoric acid, iron phosphate and manganese phosphoric acid), silicate and inorganic oxide etc.General preparation technology mixes ferromagnetic powder with insulating compound and binding agent, die forming subsequently, and last heat treatment obtains powder core.As " a kind of preparation method of high performance nano-crystal powder core " (CN102709015A) patented technology take sodium metasilicate and prepare nanocrystalline magnetic core as binding agent, as a kind of inorganic binder, although sodium metasilicate environmental protection, the powder core intensity of preparation is high, but because the decomposition of sodium metasilicate can cause crackle to produce, and powder core comprehensive magnetic can be not good, particularly power loss promotes, and can not meet industry standard." a kind of soft magnetic metal powder is inorganic insulation bonding agent and preparation method thereof for core " (CN101089108A) patented technology directly utilizes inorganic oxide to carry out insulating wrapped to iron-based soft magnetic powder surface, but, ferromagnetic powder and insulating compound are simply mixed and be difficult to guarantee that each ferromagnetic particle surface can be coated last layer insulating compound, ferromagnetic particle is easily reunited, cause insulating wrapped agent skewness, the poor insulativity of product, poor stability, quality is unstable and iron loss is higher.In addition, ferromagnetic powder is carried out under oxidizing atmosphere to high-temperature oxydation, make powder surface generate oxide insulating film, also can increase substantially its resistivity.But the more difficult control of THICKNESS CONTROL condition of the even problem of oxidation of this technology and insulation film.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, object is to provide a kind of small investment, technique is simple, efficiency is high a kind of preparation method with the ferrous alloy powder core of nucleocapsid heterostructure, the ferrous alloy powder core with nucleocapsid heterostructure of preparing by the method not only has high saturation induction density and density, can also improve insulation property and reduce eddy current loss.
For reaching above-mentioned object, the technical solution used in the present invention is following steps:
The first step, first the inorganic oxide powder of the iron(-)base powder of 80 ~ 95wt% and 5 ~ 20wt% is mixed, then ball milling 1 ~ 5h under inert gas shielding, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.01 ~ 0.15MPa, pass into inert gas to normal pressure; Then the heating rate with 50 ~ 100 ℃/min is warming up to 900 ~ 1250 ℃, with the compression rate equating, graphite jig is applied to pressure to 20 ~ 50MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under inert gas shielding, under 900 ~ 1250 ℃ of conditions, be incubated 5 ~ 30min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 30 ~ 50 ℃/min under inert gas shielding are cooled to 400 ~ 500 ℃, are cooled to the pressure during 400 ~ 500 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The particle diameter of described iron(-)base powder is less than 100 μ m; The Si content of iron(-)base powder is 0.1 ~ 14wt%, and Al content is 0.01 ~ 8wt%.
Described inorganic oxide powder particle diameter is less than 100nm; Inorganic oxide powder is SiO
2powder, MgO powder and Al
2o
3more than one in powder.
The technological parameter of described ball milling is: ball material mass ratio is (10 ~ 20) ︰ 1; The rotating speed of ball mill is 100 ~ 500r/min.
Described inert gas is argon gas or is nitrogen.
Owing to adopting technique scheme, the present invention has the following advantages:
using plasma activated sintering technology of the present invention makes take the ferrous alloy powder core with nucleocapsid heterostructure that ferrous alloy is shell as core and the inorganic oxide of take.Sintering time only has 5 ~ 30min, is only 1/4 ~ 1/20 of existing heat treatment time, simple to operate, without adding binding agent and release agent, has reduced production cost and investment, has improved production efficiency.
the present invention adopts SiO
2powder, MgO powder and Al
2o
3more than one oxides in powder are coated iron(-)base powder as insulating compound, avoided the use of organic insulation agent and binding agent in prior art, can under higher temperature, to thering is the ferrous alloy composite powder of nucleocapsid heterostructure, heat-treat, the density of the ferrous alloy powder core with nucleocapsid heterostructure obtaining is high, Heat stability is good, can under higher ambient temperature, work for a long time.
using plasma activated sintering technology of the present invention, can obtain relative density and surpass 90% the ferrous alloy powder core with nucleocapsid heterostructure, apparently higher than the powder core density of prior art gained.The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present invention is after testing: saturation induction density is 147 ~ 176emu/g; During 100kHz, magnetic permeability μ=104.8 ~ 126.4 of powder core; When magnetic permeability drops to 50%, direct current biasing field is 39.6 ~ 43.7Oe; During 100kHz/50mt, the volume ratio loss P of powder core
cv=175 ~ 192mW/cm
3.Therefore it is high that gained has the content of ferromagnetic substance in the ferrous alloy powder core unit volume of nucleocapsid heterostructure, saturated magnetic strength is high.
iron(-)base powder in the ferrous alloy powder core with nucleocapsid heterostructure prepared by the present invention is evenly coated by inorganic insulation layer, between iron(-)base powder, by inorganic insulation layer, isolated, the eddy current having in the ferrous alloy powder core of nucleocapsid heterostructure is limited in insulating wrapped district, and eddy current loss is low.
Therefore, the present invention has reduced investment, technique is simple, production efficiency is high and production cost is low feature, the saturation induction density of the prepared ferrous alloy powder core with nucleocapsid heterostructure is high, density is high, good insulation preformance, eddy current loss is low and Heat stability is good, can compared with under high ambient temperature, work for a long time.
Accompanying drawing explanation
Fig. 1 is the prepared a kind of XRD collection of illustrative plates with the ferrous alloy powder core of nucleocapsid heterostructure of the present invention;
Fig. 2 is the section SEM figure of the ferrous alloy powder core with nucleocapsid heterostructure shown in Fig. 1;
Fig. 3 is the magnetic hysteresis loop figure of the ferrous alloy powder core with nucleocapsid heterostructure shown in Fig. 1.
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, the raw material unification first this embodiment being related to is described below, and in embodiment, repeats no more:
The particle diameter of described iron(-)base powder is less than 100 μ m; The Si content of iron(-)base powder is 0.1 ~ 14wt%, and Al content is 0.01 ~ 8wt%.
Described SiO
2powder, MgO powder and Al
2o
3the particle diameter of powder is less than 100nm.
embodiment 1
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by the SiO of the iron(-)base powder of 80 ~ 85wt% and 15 ~ 20wt%
2powder mixes, ball milling 1 ~ 1.5h under argon shield then, and ball material mass ratio is that (10 ~ 12) ︰ 1, the rotating speed of ball mill is 100 ~ 200r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.01 ~ 0.05MPa, pass into argon gas to normal pressure; Then the heating rate with 50 ~ 60 ℃/min is warming up to 900 ~ 950 ℃, with the compression rate equating, graphite jig is applied to pressure to 20 ~ 25MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under argon shield, under 900 ~ 950 ℃ of conditions, be incubated 5 ~ 10min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 30 ~ 35 ℃/min under argon shield are cooled to 400 ~ 450 ℃, are cooled to the pressure during 400 ~ 450 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 148 ~ 157emu/g;
(2) during 100kHz, magnetic permeability μ=105.1 ~ 111.3 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 41.4 ~ 42.1Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=175 ~ 177mW/cm
3.
embodiment 2
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first the MgO powder of the iron(-)base powder of 85 ~ 90wt% and 10 ~ 15wt% is mixed; then ball milling 1.5 ~ 2h under argon shield; ball material mass ratio is (12 ~ 14) ︰ 1; the rotating speed of ball mill is 200 ~ 300r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.05 ~ 0.10MPa, pass into argon gas to normal pressure; Then the heating rate with 60 ~ 70 ℃/min is warming up to 950 ~ 1000 ℃, with the compression rate equating, graphite jig is applied to pressure to 25 ~ 30MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under argon shield, under 950 ~ 1000 ℃ of conditions, be incubated 10 ~ 15min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 35 ~ 40 ℃/min under argon shield are cooled to 450 ~ 500 ℃, are cooled to the pressure during 450 ~ 500 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 156 ~ 166emu/g;
(2) during 100kHz, magnetic permeability μ=112.5 ~ 118.8 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 40.8 ~ 41.3Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=179 ~ 182mW/cm
3.
embodiment 3
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by the Al of the iron(-)base powder of 90 ~ 95wt% and 5 ~ 10wt%
2o
3powder mixes, ball milling 2 ~ 2.5h under argon shield then, and ball material mass ratio is that (14 ~ 16) ︰ 1, the rotating speed of ball mill is 300 ~ 400r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.10 ~ 0.15MPa, pass into nitrogen to normal pressure; Then the heating rate with 70 ~ 80 ℃/min is warming up to 1000 ~ 1050 ℃, with the compression rate equating, graphite jig is applied to pressure to 30 ~ 35MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under nitrogen protection, under 1000 ~ 1050 ℃ of conditions, be incubated 15 ~ 20min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 40 ~ 45 ℃/min under nitrogen protection are cooled to 410 ~ 420 ℃, are cooled to the pressure during 410 ~ 420 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 167 ~ 176emu/g;
(2) during 100kHz, magnetic permeability μ=119.2 ~ 126.4 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 39.8 ~ 40.2Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=184 ~ 186mW/cm
3.
embodiment 4
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by the SiO of the iron(-)base powder of 80 ~ 82wt% and 18 ~ 20wt%
2powder and MgO powder mix, ball milling 2.5 ~ 3h under argon shield then, and ball material mass ratio is that (16 ~ 18) ︰ 1, the rotating speed of ball mill is 400 ~ 500r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.01 ~ 0.04MPa, pass into nitrogen to normal pressure; Then the heating rate with 80 ~ 90 ℃/min is warming up to 1050 ~ 1100 ℃, with the compression rate equating, graphite jig is applied to pressure to 35 ~ 40MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under nitrogen protection, under 1050 ~ 1100 ℃ of conditions, be incubated 20 ~ 25min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 45 ~ 50 ℃/min under nitrogen protection are cooled to 440 ~ 450 ℃, are cooled to the pressure during 440 ~ 450 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 147 ~ 152emu/g;
(2) during 100kHz, magnetic permeability μ=104.8 ~ 107.6 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 39.6 ~ 39.9Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=176 ~ 179mW/cm
3.
embodiment 5
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by the SiO of the iron(-)base powder of 84 ~ 87wt% and 13 ~ 16wt%
2powder and Al
2o
3powder mixes, ball milling 3 ~ 3.5h under nitrogen protection then, and ball material mass ratio is that (18 ~ 20) ︰ 1, the rotating speed of ball mill is 100 ~ 150r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.05 ~ 0.08MPa, pass into argon gas to normal pressure; Then the heating rate with 90 ~ 100 ℃/min is warming up to 1100 ~ 1150 ℃, with the compression rate equating, graphite jig is applied to pressure to 40 ~ 45MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under argon shield, under 1100 ~ 1150 ℃ of conditions, be incubated 25 ~ 30min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 30 ~ 36 ℃/min under argon shield are cooled to 460 ~ 480 ℃, are cooled to the pressure during 460 ~ 480 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 155 ~ 161emu/g;
(2) during 100kHz, magnetic permeability μ=110.0 ~ 114.8 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 42.7 ~ 43.5Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=178 ~ 183mW/cm
3.
embodiment 6
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by MgO powder and the Al of the iron(-)base powder of 89 ~ 92wt% and 8 ~ 11wt%
2o
3powder mixes, ball milling 3.5 ~ 4h under nitrogen protection then, and ball material mass ratio is that (15 ~ 20) ︰ 1, the rotating speed of ball mill is 200 ~ 250r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.10 ~ 0.13MPa, pass into argon gas to normal pressure; Then the heating rate with 55 ~ 65 ℃/min is warming up to 1150 ~ 1200 ℃, with the compression rate equating, graphite jig is applied to pressure to 45 ~ 50MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under argon shield, under 1150 ~ 1200 ℃ of conditions, be incubated 5 ~ 8min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 42 ~ 48 ℃/min under argon shield are cooled to 490 ~ 500 ℃, are cooled to the pressure during 490 ~ 500 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 165 ~ 170emu/g;
(2) during 100kHz, magnetic permeability μ=116.6 ~ 121.1 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 41.5 ~ 42.0Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=184 ~ 192mW/cm
3.
embodiment 7
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by the SiO of the iron(-)base powder of 92 ~ 95wt% and 5 ~ 8wt%
2powder, MgO powder and Al
2o
3powder mixes, ball milling 4 ~ 4.5h under nitrogen protection then, and ball material mass ratio is that (10 ~ 15) ︰ 1, the rotating speed of ball mill is 300 ~ 350r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.12 ~ 0.15MPa, pass into nitrogen to normal pressure; Then the heating rate with 75 ~ 85 ℃/min is warming up to 1200 ~ 1250 ℃, with the compression rate equating, graphite jig is applied to pressure to 22 ~ 27MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under nitrogen protection, under 1200 ~ 1250 ℃ of conditions, be incubated 8 ~ 12min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 48 ~ 50 ℃/min under nitrogen protection are cooled to 430 ~ 450 ℃, are cooled to the pressure during 430 ~ 450 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 168 ~ 176emu/g;
(2) during 100kHz, magnetic permeability μ=119.2 ~ 126.3 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 43.2 ~ 43.7Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=188 ~ 191mW/cm
3.
embodiment 8
A kind of ferrous alloy powder core with nucleocapsid heterostructure and preparation method thereof.The preparation method of the present embodiment is:
The first step, first by the SiO of the iron(-)base powder of 87 ~ 89wt% and 11 ~ 13wt%
2powder mixes, ball milling 4.5 ~ 5h under nitrogen protection then, and ball material mass ratio is that (16 ~ 18) ︰ 1, the rotating speed of ball mill is 400 ~ 450r/min, makes the ferrous alloy composite powder with nucleocapsid heterostructure.
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.08 ~ 0.10MPa, pass into nitrogen to normal pressure; Then the heating rate with 95 ~ 100 ℃/min is warming up to 950 ~ 1050 ℃, with the compression rate equating, graphite jig is applied to pressure to 35 ~ 42MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization.
The 3rd step, under nitrogen protection, under 950 ~ 1050 ℃ of conditions, be incubated 28 ~ 30min, the pressure between soak, graphite jig being applied is constant.
The 4th step, the rate of temperature fall with 36 ~ 42 ℃/min under nitrogen protection are cooled to 470 ~ 490 ℃, are cooled to the pressure during 470 ~ 490 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig.
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
The ferrous alloy powder core with nucleocapsid heterostructure prepared by the present embodiment is after testing:
(1) saturation induction density is 156 ~ 163emu/g;
(2) during 100kHz, magnetic permeability μ=111.2 ~ 117.3 of powder core;
(3), when magnetic permeability drops to 50%, direct current biasing field is 41.5 ~ 42.6Oe;
(4) during 100kHz/50mt, the volume ratio loss P of powder core
cv=177 ~ 181mW/cm
3.
This embodiment compared with prior art has following good effect:
this embodiment using plasma activated sintering technology makes take the ferrous alloy powder core with nucleocapsid heterostructure that ferrous alloy is shell as core and the inorganic oxide of take.Sintering time only has 5 ~ 30min, is only 1/4 ~ 1/20 of existing heat treatment time, simple to operate, without adding binding agent and release agent, has reduced production cost and investment, has improved production efficiency.
this embodiment adopts SiO
2powder, MgO powder and Al
2o
3more than one oxides in powder are coated iron(-)base powder as insulating compound, and the prepared ferrous alloy powder core with nucleocapsid heterostructure of implementation column 1 as shown in Figure 1 shows and only has SiO in its XRD collection of illustrative plates
2with two kinds of thing phases of ferro-silicium.Avoided the use of organic insulation agent and binding agent in prior art, can under higher temperature, to thering is the ferrous alloy composite powder of nucleocapsid heterostructure, heat-treat, the density of the ferrous alloy powder core with nucleocapsid heterostructure obtaining is high, Heat stability is good, can under higher ambient temperature, work for a long time.
this embodiment using plasma activated sintering technology, can obtain relative density and surpass 90% the ferrous alloy powder core with nucleocapsid heterostructure, apparently higher than the powder core density of prior art gained.The prepared ferrous alloy powder core with nucleocapsid heterostructure of implementation column 1 as shown in Figure 2, its saturation induction density is 148 ~ 157emu/g.The ferrous alloy powder core with nucleocapsid heterostructure prepared by this embodiment is after testing: saturation induction density is 147 ~ 176emu/g; During 100kHz, magnetic permeability μ=104.8 ~ 126.4 of powder core; When magnetic permeability drops to 50%, direct current biasing field is 39.6 ~ 43.7Oe; During 100kHz/50mt, the volume ratio loss P of powder core
cv=175 ~ 192mW/cm
3.Therefore it is high that gained has the content of ferromagnetic substance in the ferrous alloy powder core unit volume of nucleocapsid heterostructure, saturated magnetic strength is high.
iron(-)base powder in the ferrous alloy powder core with nucleocapsid heterostructure prepared by this embodiment is evenly coated by inorganic insulation layer, the prepared ferrous alloy powder core with nucleocapsid heterostructure of implementation column 1 as shown in Figure 3, its SEM figure shows in the ferrous alloy powder core with nucleocapsid heterostructure that ferro-silicium powder is by SiO
2evenly coated, between ferro-silicium powder by SiO
2isolation, the eddy current having in the ferrous alloy powder core of nucleocapsid heterostructure is limited in insulating wrapped district, and eddy current loss is low.
Therefore, this embodiment has reduced investment, technique is simple, production efficiency is high and production cost is low feature, the saturation induction density of the prepared ferrous alloy powder core with nucleocapsid heterostructure is high, density is high, good insulation preformance, eddy current loss is low and Heat stability is good, can compared with under high ambient temperature, work for a long time.
Claims (6)
1. a preparation method with the ferrous alloy powder core of nucleocapsid heterostructure, is characterized in that described preparation method is:
The first step, first the inorganic oxide powder of the iron(-)base powder of 80 ~ 95wt% and 5 ~ 20wt% is mixed, then ball milling 1 ~ 5h under inert gas shielding, makes the ferrous alloy composite powder with nucleocapsid heterostructure;
Second step, pack the described ferrous alloy composite powder with nucleocapsid heterostructure into graphite jig, more described graphite jig is placed in to plasma activated sintering stove, be evacuated to 0.01 ~ 0.15MPa, pass into inert gas to normal pressure; Then the heating rate with 50 ~ 100 ℃/min is warming up to 900 ~ 1250 ℃, with the compression rate equating, graphite jig is applied to pressure to 20 ~ 50MPa, and the beginning and ending time of intensification is with identical to the beginning and ending time of graphite jig pressurization;
The 3rd step, under inert gas shielding, under 900 ~ 1250 ℃ of conditions, be incubated 5 ~ 30min, the pressure between soak, graphite jig being applied is constant;
The 4th step, the rate of temperature fall with 30 ~ 50 ℃/min under inert gas shielding are cooled to 400 ~ 500 ℃, are cooled to the pressure during 400 ~ 500 ℃, graphite jig being applied constant; Then with stove, naturally cool to room temperature, with stove nature cooling period with the rate of pressure reduction that equates the pressure drop to 0 to graphite jig;
The 5th step, come out of the stove, the demoulding, must have the ferrous alloy powder core of nucleocapsid heterostructure.
2. the preparation method with the ferrous alloy powder core of nucleocapsid heterostructure according to claim 1, is characterized in that the particle diameter of described iron(-)base powder is less than 100 μ m; The Si content of iron(-)base powder is 0.1 ~ 14wt%, and Al content is 0.01 ~ 8wt%.
3. the preparation method with the ferrous alloy powder core of nucleocapsid heterostructure according to claim 1, is characterized in that described inorganic oxide powder particle diameter is less than 100nm; Inorganic oxide powder is SiO
2powder, MgO powder and Al
2o
3more than one in powder.
4. the preparation method with the ferrous alloy powder core of nucleocapsid heterostructure according to claim 1, is characterized in that the technological parameter of described ball milling is: ball material mass ratio is for (10 ~ 20) ︰ 1, the rotating speed of ball mill is 100 ~ 500r/min.
5. the preparation method with the ferrous alloy powder core of nucleocapsid heterostructure according to claim 1, is characterized in that described inert gas is argon gas or is nitrogen.
6. a ferrous alloy powder core with nucleocapsid heterostructure, the ferrous alloy powder core described in it is characterized in that with nucleocapsid heterostructure is according to the prepared ferrous alloy powder core with nucleocapsid heterostructure of preparation method of the ferrous alloy powder core with nucleocapsid heterostructure described in any one in claim 1 ~ 5.
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