CN101246773A - High-efficiency soft magnetic material and method for producing the same - Google Patents
High-efficiency soft magnetic material and method for producing the same Download PDFInfo
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- CN101246773A CN101246773A CNA2007100638436A CN200710063843A CN101246773A CN 101246773 A CN101246773 A CN 101246773A CN A2007100638436 A CNA2007100638436 A CN A2007100638436A CN 200710063843 A CN200710063843 A CN 200710063843A CN 101246773 A CN101246773 A CN 101246773A
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Abstract
The invention relates to a highly efficient soft magnetic material and the preparing method thereof. The soft magnetic material is composed of metal soft magnetic material and soft magnetic ferrite, the metal soft magnetic material is composed of at least one selected from Fe-Ni-Me system (Me is one or more than two selected form Cu, Cr, Nb, V, W, Si, Pd, Zn, Al, Ti and Mn), Fe-Co system, Fe-Co-V system, Fe-Al system and Fe-Al-Me system (Me is one or more than two selected form Co, Cr and Mo), the soft magnetic ferrite is composed of at least one selected form Mn-Zn system, Ni-Zn system, Li-Zn system, Cu-Zn system and Mg-Zn system soft magnetic ferrites. The preparing method of the soft magnetic material comprises the steps of: cold pressing, and sintering, hot pressing or spark plasma sintering. The soft magnetic material does not have the drawbacks of low resistivity of the metal soft magnetic and low magnetic strength of the ferrite, as well as keeps the superior properties of the metal soft magnetic and low magnetic strength of the ferrite.
Description
Technical field
The invention belongs to field of magnetic material, relate to a kind of composition and preparation method of the soft magnetic material of forming by soft magnetic metal powder and soft magnetic ferrite.
Background technology
Soft magnetic material commonly used now mainly contains electrical pure iron, silicon steel sheet, iron-nickel alloy, ferrite and amorphous and nanocrystalline material.We have successively carried out practical application for electrical pure iron, silicon steel sheet, iron-nickel alloy, ferrite and amorphous, studies show that existing permeability magnetic material is difficult to satisfy simultaneously the instructions for use of mechanical property, magnetic performance and electric property.
Electrical pure iron magnetic performance and mechanical property excellence (magnetic permeability height, saturation induction density height (～2T), mechanical strength height), but electric property poor (resistivity is low), eddy current loss is big under alternating field, can't satisfy actual use; Silicon steel sheet magnetic performance and electric property excellence (high saturation induction density, high magnetic permeability, high resistivity are arranged), but poor mechanical property (compression strength is low); Iron-nickel alloy magnetic permeability height, the saturation induction density height, yielding, and anti-eddy current is limited in one's ability, though take to reduce the eddy current loss measure by lamination etc., can raise the efficiency to a certain extent, but also obviously influence power and efficient, is difficult to satisfy actual needs; The anti-eddy current ability of ferrite is strong, but saturation induction density low (～0.6T), the design that influences magnetic circuit system with effectively use, for the bias magnetic field optimal design bigger challenge and difficulty have been proposed, influence is selected to use; Amorphous and nanocrystalline not withstand voltage, mechanical loss is big, can't satisfy actual use.
Because soft magnetic material generally is used for the environment that vibration proof impacts, for the research unit of soft magnetic material, what often pursue is the magnetics parameter and the electrical parameter of material, wishes that magnetic permeability is high as far as possible, eddy current loss is little, pursue electromagnetic conversion efficient height, do not have enough attention for mechanics parameter.Because in the applied acoustics research of novel sonar transducer, what usually use is the existing soft magnetic material in domestic industry market, be subjected to the limitation of existing soft magnetic material, not specially in conjunction with the real needs and the hand-in-glove of associated materials unit of application study, make the performance of ultra-magnetic telescopic drive vibrator not to be not fully exerted and electricity-magnetic-the machine conversion efficiency is on the low side (generally being lower than 40%).
Chinese patent CN96120255.6 discloses a kind of biphase nanocrystalline iron based soft magnetic materials and preparation method thereof.Adopt the method for single roller Quench obtain amorphous thin ribbon again heat treatment obtain FeZrNbSiB and FeYNbSiB biphase peritectic alloy, the soft magnet performance and the toughness of this material are better, but intensity and electric property are relatively poor.
Chinese patent CN03128171.0 discloses a kind of preparation method of soft magnetic material.Soft magnetic material comprises straight iron powder, insulating compound and lubricant, and production technology is made up of mixed powder and sintering.But the composition of this invention and technology are only pursued magnetic permeability and eddy current loss, have ignored mechanical property and electric property.
In order further to improve the combination property of magnetically soft alloy, enlarge the range of application of magnetically soft alloy, be badly in need of the soft magnetic material of a kind of new and effective energy of development.
Summary of the invention
The present invention seeks to: guaranteeing between magnetic performance and electric property, to carry out overall balance under the prerequisite of mechanical property, a kind of high strength, anti-eddy current, novel soft magnetic material that soft magnet performance is good are provided.
In order to achieve the above object, the present invention adopts following embodiment:
The present invention relates to a kind of soft magnetic material, it is characterized in that: this soft magnetic material is made up of soft magnetic metal powder and soft magnetic ferrite powder, wherein (Me is Cu to metal soft magnetic material by Fe-Ni-Me system, Cr, Nb, V, W, Si, Pd, Zn, Al, Ti, among the Mn one or more), Fe-Co system, Fe-Co-V system, Fe-Al system, (Me is Co in Fe-Al-Me system, Cr, among the Mo one or more) at least a composition in, soft magnetic ferrite powder by Mn-Zn is, Ni-Zn system, Li-Zn system, Cu-Zn system, at least a composition in the Mg-Zn series soft magnetic ferrite.
The preparation technology of soft magnetic material of the present invention may further comprise the steps:
1) two kinds of soft magnetic powder mixed processes.Metal soft magnetic alloy powder and soft magnetic ferrite powder are mixed.
2) soft magnetic composite powder sintering circuit.A kind of in sintering, hot pressing, the discharge plasma sintering again after can selecting to cold pressing.
After colding pressing again the operation of sintering be characterised in that: first cold moudling, added pressure are 10～30MPa, sintering in hydrogen atmosphere then, earlier at 400 ℃～500 ℃ pre-burning 1～3h, again at 900 ℃～1200 ℃, sintering 1～5h.
Hot pressing process is characterized in that: at 800 ℃～1000 ℃ hot pressing 10min～1h, with the stove cooling, added pressure is 10～30MPa to soft magnetic composite powder during hot pressing then in mould.
The discharge plasma sintering operation is characterized in that: soft magnetic composite powder is at 600 ℃～900 ℃ sintering 5min～15min, is as cold as 100 ℃ and comes out of the stove with 20 ℃/h～30 ℃/cooling rate of h then, and added pressure is 20～60MPa during discharge plasma sintering.
3) annealing in process operation is characterized in that: in the hydrogen atmosphere of 100～150Pa, 2～5h anneals in 1000 ℃～1200 ℃ scopes.
The used soft magnetic metal powder market of the present invention is on sale, and " at% " represents atomic percent.
Described soft magnetic metal powder, its particle size are 10～100 μ m.
Described soft magnetic ferrite powder, its particle size are 10～120 μ m.
The advantage of soft magnetic material of the present invention is: possess good soft magnet performance and electric property on the one hand under bias magnetic field and alternating magnetic field, promptly has high magnetic permeability, high resistivity and high saturation magnetic field intensity, can improve magnetic efficiency, reduce eddy current loss, have on the other hand and can guarantee to carry out the required mechanical property of energy delivery, be that compression strength height, in-fighting are little, can reduce the mechanical oscillation loss.
The advantage of preparation soft magnetic material technology of the present invention is: technical process is simple, and the performance of material is convenient to control, is fit to suitability for industrialized production, and is convenient to moulding, can prepare complex-shaped sample.
Embodiment
Below the invention will be further described with example.Protection range of the present invention is not subjected to the restriction of these embodiment.
The 1st embodiment:
Composition be 90% Fe-Ni-Cu powder and 10% the Mn-Zn ferrite (composition of Fe-Ni-Cu is as follows: Ni50wt%, Fe46wt%, Cu 4wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt cold pressing after sintering process again, at first, Fe-Ni-Cu powder with 90% and 10% Mn-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 1.
The performance of sample under the different sintering process of table 1
Annotate: μ
iBe initial permeability, μ
mBe maximum permeability, μ ' is an elastic magnetic inductivity, B
sBe saturated magnetic strength, E is a modulus of elasticity, and σ is a compression strength, and ρ is a resistivity
The 2nd embodiment:
Composition be 80% Fe-Ni-Nb powder and 20% the Ni-Zn ferrite (composition of Fe-Ni-Nb is as follows: Ni49wt%, Fe49wt%, Nb2wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt cold pressing after sintering process again, at first, Fe-Ni-Nb powder with 80% and 20% Ni-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 2.
The performance of sample under the different sintering process of table 2
The 3rd embodiment:
With the Fe-Ni-Cu powder of different proportion and Mn-Zn ferrite powder (composition of Fe-Ni-Cu is as follows: Ni50wt%, Fe26wt%, Cu 4wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 3.
The performance of table 3 heterogeneity sample
The 4th embodiment:
With the Fe-Ni-Nb powder of different proportion and Ni-Zn ferrite powder (composition of Fe-Ni-Nb is as follows: Ni49wt%, Fe49wt%, Nb2wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 4.
The performance of table 4 heterogeneity sample
The 5th embodiment:
Composition be 50% Fe-Ni-Cu-Nb powder and 50% the Mn-Zn ferrite (composition of Fe-Ni-Cu-Nb is as follows: Ni49wt%, Fe46wt%, Cu3wt%, Nb2wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Ni-Cu-Nb powder with 50% and 50% Mn-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 5.
The performance of sample under the different discharge plasma sintering process of table 5
The 6th embodiment:
Composition be 70% Fe-Ni-Cu-Nb powder and 30% the Ni-Zn ferrite (composition of Fe-Ni-Cu-Nb is as follows: Ni49wt%, Fe46wt%, Cu3wt%, Nb2wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Ni-Cu-Nb powder with 70% and 30% Ni-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 6.
The performance of sample under the different discharge plasma sintering process of table 6
The 7th embodiment:
Composition be 90% Fe-Co powder and 10% the Mn-Zn ferrite (composition of Fe-Co is as follows: Co50wt%, Fe50wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt cold pressing after sintering process again, at first, Fe-Co powder with 90% and 10% Mn-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 7.
The performance of sample under the different sintering process of table 7
The 8th embodiment:
Composition be 80% Fe-Co powder and 20% the Ni-Zn ferrite (composition of Fe-Co is as follows: Co50wt%, Fe50wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt cold pressing after sintering process again, at first, Fe-Co powder with 80% and 20% Ni-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 8.
The performance of sample under the different sintering process of table 8
The 9th embodiment:
With the Fe-Co powder of different proportion and Mn-Zn ferrite powder (composition of Fe-Co is as follows: Co50wt%, Fe50wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 9.
The performance of table 9 heterogeneity sample
The 10th embodiment:
With the Fe-Co-V powder of different proportion and Ni-Zn ferrite powder (composition of Fe-Co-V is as follows: Co49wt%, Fe49wt%, V2wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 10.
The performance of table 10 heterogeneity sample
The 11st embodiment:
Composition be 50% Fe-Co-V powder and 50% the Mn-Zn ferrite (composition of Fe-Co-V is as follows: Co49wt%, Fe49wt%, V2wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Co-V powder with 50% and 50% Mn-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 11.
The performance of sample under the different discharge plasma sintering process of table 11
The 12nd embodiment:
Composition be 70% Fe-Co-V powder and 30% the Ni-Zn ferrite (composition of Fe-Co-V is as follows: Co49wt%, Fe49wt%, V2wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Co-V powder with 70% and 30% Ni-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 12.
The performance of sample under the different discharge plasma sintering process of table 12
The 13rd embodiment:
Composition be 90% Fe-Al powder and 10% the Mn-Zn ferrite (composition of Fe-Al is as follows: Al12wt%, Fe88wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt cold pressing after sintering process again, at first, Fe-Al powder with 90% and 10% Mn-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 13.
The performance of sample under the different sintering process of table 13
The 14th embodiment:
Composition be 80% Fe-Al powder and 20% the Ni-Zn ferrite (composition of Fe-Al is as follows: Al12wt%, Fe88wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt cold pressing after sintering process again, at first, Fe-Al powder with 80% and 20% Ni-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in table 14.
The performance of sample under the different sintering process of table 14
The 15th embodiment:
With the Fe-Al powder of different proportion and Mn-Zn ferrite powder (composition of Fe-50Ni is as follows: Al12wt%, Fe88wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is as shown in Table 15.
The performance of table 15 heterogeneity sample
The 16th embodiment:
With the Fe-Al powder of different proportion and Ni-Zn ferrite powder (composition of Fe-Al is as follows: Al12wt%, Fe88wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 16.
The performance of table 16 heterogeneity sample
The 17th embodiment:
Composition be 50% Fe-Al powder and 50% the Mn-Zn ferrite (composition of Fe-Al is as follows: Al12wt%, Fe88wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Al powder with 50% and 50% Mn-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 17.
The performance of sample under the different discharge plasma sintering process of table 17
The 18th embodiment:
Composition be 70% Fe-Al powder and 30% the Ni-Zn ferrite (composition of Fe-Al is as follows: Al12wt%, Fe88wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Al powder with 70% and 30% Ni-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 18.
The performance of sample under the different discharge plasma sintering process of table 18
The 19th embodiment:
Composition be 90% Fe-Al-Co powder and 10% the Mn-Zn ferrite (composition of Fe-Al-Co is as follows: Al12wt%, Fe86wt%, Co2wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt cold pressing after sintering process again, at first, Fe-Al-Co powder with 90% and 10% Mn-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 19.
The performance of sample under the different sintering process of table 19
The 20th embodiment:
Composition be 80% Fe-Al-Co powder and 20% the Ni-Zn ferrite (composition of Fe-Al-Co is as follows: Al12wt%, Fe86wt%, Co2wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt cold pressing after sintering process again, at first, Fe-Al-Co powder with 80% and 20% Ni-Zn ferrite powder mix the back and are pressing compression moulding on the model machine, added pressure is 20MPa in cold pressure procedure; Sintering in sintering furnace is evacuated to 10 earlier during sintering again
-3Below the Pa, charge into the hydrogen of 122Pa again,, in hydrogen atmosphere, behind 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃ sintering 3h, be cooled to 200 ℃ respectively again and come out of the stove with stove earlier at 450 ℃ of pre-burning 3h; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 20.
The performance of sample under the different sintering process of table 20
The 21st embodiment:
With the Fe-Al-Co powder of different proportion and Mn-Zn ferrite powder (composition of Fe-Al-Co is as follows: Al12wt%, Fe86wt%, Co2wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20Mpa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 21.
The performance of table 21 heterogeneity sample
The 22nd embodiment:
With the Fe-Al-Mo powder of different proportion and Ni-Zn ferrite powder (composition of Fe-Al-Mo is as follows: Al12wt%, Fe84wt%, Mo4wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%) adopt the heat pressing process moulding, at first, at 930 ℃ of hot pressing 0.5h, the argon gas that charges in the hot pressing is 100Pa with the soft magnetism composite magnetic powder that mixes, and added pressure is 20MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 22.
The performance of table 22 heterogeneity sample
The 23rd embodiment:
Composition be 50% Fe-Al-Mo powder and 50% the Mn-Zn ferrite (composition of Fe-Al-Mo is as follows: Al12wt%, Fe84wt%, Mo4wt%, the ferritic composition of Mn-Zn is as follows: MnO15at%, ZnO15at%, Fe
2O
370at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Si-Al powder with 50% and 50% Mn-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 23.
The performance of sample under the different discharge plasma sintering process of table 23
The 24th embodiment:
Composition be 70% Fe-Al-Mo powder and 30% the Ni-Zn ferrite (composition of Fe-Al-Mo is as follows: Al12wt%, Fe84wt%, Mo4wt%, the ferritic composition of Ni-Zn is as follows: NiO30at%, ZnO20at%, Fe
2O
350at%), adopt discharge plasma sintering process, at first, after mixing, Fe-Al-Mo powder with 70% and 30% Ni-Zn ferrite powder carry out discharge plasma sintering, being as cold as 100 ℃ with the cooling rate of 100 ℃/h respectively behind 600 ℃, 700 ℃, 800 ℃, 900 ℃ sintering 5min in argon gas atmosphere comes out of the stove, during discharge plasma sintering, the argon gas that charges into is 100Pa, and added pressure is 35MPa; Carry out annealing in process then, during annealing, be evacuated to 10 earlier
-3Below the Pa, charge into the hydrogen of 100Pa again, at 1100 ℃ of annealing 3h, Quench is to room temperature then in hydrogen atmosphere; Soft magnet performance, electric property and the mechanical property of last test sample, its result is shown in table 24.
The performance of sample under the different discharge plasma sintering process of table 24
Claims (12)
1. high-efficiency soft magnetic material, it is characterized in that: it is made up of soft magnetic metal powder and soft magnetic ferrite powder, and wherein, the ratio of soft magnetic metal powder is 50wt%～90wt%, and surplus is soft magnetic ferrite powder.
2. a kind of high-efficiency soft magnetic material according to claim 1, it is characterized in that: described soft magnetic metal powder, by at least a composition the in Fe-Ni-Me system (Me is one or more among Cu, Cr, Nb, V, W, Si, Pd, Zn, Al, Ti, the Mn), Fe-Co system, Fe-Co-V system, Fe-Al system, the Fe-Al-Me system (Me is one or more among Co, Cr, the Mo).
3. a kind of high-efficiency soft magnetic material according to claim 1 and 2 is characterized in that: described soft magnetic ferrite powder is by at least a composition the in Mn-Zn system, Ni-Zn system, Li-Zn system, Cu-Zn system, the Mg-Zn series soft magnetic ferrite.
4. a kind of high-efficiency soft magnetic material according to claim 2 is characterized in that: described soft magnetic metal powder, its particle size are 10～100 μ m.
5. according to claim 3 high-efficiency soft magnetic material, it is characterized in that: described soft magnetic ferrite powder, its particle size are 10～120 μ m.
6. the preparation method of soft magnetic material according to claim 1, it is characterized in that: it comprises mixed powder, sintering, the several operations of annealing in process.
7. the preparation method of soft magnetic material according to claim 6, it is characterized in that: described mixed powder is that the soft magnetic metal powder is mixed with soft magnetic ferrite powder, the soft magnetic composite powder that preparation mixes.
8. the preparation method of soft magnetic material according to claim 6 is characterized in that: sintering or hot pressing or discharge plasma sintering again after the sintering circuit of described soft magnetic material is selected to cold pressing.
9. the preparation method of soft magnetic material according to claim 8, it is characterized in that: after described the colding pressing again the operation of sintering comprise: first cold moudling, added pressure is 10～30MPa, sintering in hydrogen atmosphere then, earlier at 400 ℃～500 ℃ pre-burning 1～3h, again at 900 ℃～1200 ℃, sintering 1～5h.
10. the preparation method of soft magnetic material according to claim 8, it is characterized in that: described hot pressing process is included in the argon gas atmosphere, at 800 ℃～1000 ℃ hot pressing 10min～1h, with the stove cooling, added pressure is 10～30MPa to soft magnetic composite powder during hot pressing then in mould.
11. the preparation method of soft magnetic material according to claim 8, it is characterized in that: described discharge plasma sintering operation is included in the argon gas atmosphere, soft magnetic composite powder is at 600 ℃～900 ℃ sintering 5min～15min, be as cold as 100 ℃ and come out of the stove with 20 ℃/h～30 ℃/cooling rate of h then, added pressure is 20～60MPa during discharge plasma sintering.
12. the preparation method according to the described soft magnetic material of claim 6 is characterized in that: described annealing in process operation is included in the hydrogen atmosphere of 100～150Pa, and 2～5h anneals in 1000 ℃～1200 ℃ scopes.
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