CN106348744A - Soft magnetic ferrite material with high initial permeability and preparation method thereof - Google Patents

Soft magnetic ferrite material with high initial permeability and preparation method thereof Download PDF

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CN106348744A
CN106348744A CN201610719477.4A CN201610719477A CN106348744A CN 106348744 A CN106348744 A CN 106348744A CN 201610719477 A CN201610719477 A CN 201610719477A CN 106348744 A CN106348744 A CN 106348744A
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soft magnetic
magnetic ferrite
high initial
initial permeability
principal component
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王久如
瞿德林
李丛俊
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/2608Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
    • C04B35/2633Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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Abstract

The invention disclsoes a soft magnetic ferrite material with high initial permeability. The soft magnetic ferrite material is prepared from a main component and an auxiliary component at the mol ratio of 1 : (0.3 to 0.4), wherein the main component comprises: Fe2O3, ZnO, V2O5, MoO3 and TiO2 and the balance of nickel powder; the auxiliary component comprises: MnCo3, CaCO3, SiO2, Al2O3, Bi2O3, WO3 and Pr6O11. The invention further disclsoes a preparation method of the soft magnetic ferrite material with the high initial permeability. The soft magnetic ferrite material prepared by the preparation method has the high initial permeability.

Description

A kind of soft magnetic ferrite with high initial permeability and preparation method thereof
Technical field
The present invention relates to a kind of soft magnetic ferrite and preparation method thereof, relate in particular to a kind of the soft of high initial permeability that haveMagnetic ferrite material and preparation method thereof.
Background technology
Along with the fast development of digital communication technology and Fibre Optical Communication Technology, traditional artificial traffic equipment constantly upgradesEliminate. At electronic circuit wide-band transformer, the pulse in the fields such as ISDN(Integrated Service Digital Network), LAN, wide area network, background illumination becomesThe high magnetic conductivity ferrite magnetic core that in depressor and photovoltaic DC-to-AC converter, common mode filtering inductance is used, because transformer etc. is sent out towards miniaturizationExhibition, has therefore proposed requirements at the higher level to ferritic magnetic characteristic, particularly in the current electronic information epoch, and external environment variousElectronic interferences is day by day serious, needs ferrite to have high initial permeability, high saturated magnetic induction, high-curie temperature, high resistantResist and broadband properties.
The initial permeability of soft magnetic ferrite of the prior art cannot meet the demand of prior art, therefore needs design badlyA kind of soft magnetic ferrite with high initial permeability solves the problems of the prior art.
Summary of the invention
For solving the technical problem existing in background technology, the present invention proposes a kind of soft magnet with high initial permeabilityFerrite and preparation method thereof, the soft magnetic ferrite of preparation has the performance of high initial permeability.
A kind of soft magnetic ferrite with high initial permeability that the present invention proposes, is pressed by principal component and auxiliary elementMol ratio 1:(0.3-0.4) make;
Wherein said principal component and mass percent are calculated as by oxide:
Fe2O3:52.5-54.6wt%;
ZnO:12.5-14.5wt%;
V2O5:3.5-5.5wt%;
MoO3:1.5-3.5wt%;
TiO2:0.5-1.5wt%;
Residue is nickel powder;
Auxiliary element and molar percentage are calculated as by oxide:
MnCO3:0.01-0.03wt%;
CaCO3:0.02-0.05wt%;
SiO2:0.03-0.06wt%;
Al2O3:0.01-0.05wt%;
Bi2O3:0.005-0.015wt%;
WO3:0.001-0.005wt%;
Pr6O11:0.003-0.006wt%。
Preferably, in principal component, Fe2O3、ZnO、V2O5、MoO3And TiO2Mass percent be 52.8-54.3:12.8- 14.2:3.8-5.2:1.8-3.2:0.8-1.2。
Preferably, in auxiliary element, MnCO3、CaCO3、SiO2、Al2O3、Bi2O3、WO3And Pr6O11Mass percent be 0.015-0.025:0.03-0.04:0.04-0.05:0.02-0.04:0.008-0.012:0.002-0.004:0.004- 0.005。
Preferably, by principal component and auxiliary element 1:(0.32-0.38 in molar ratio) make, wherein said principal component andMass percent is calculated as by oxide: Fe2O3:52.8-54.3wt%;ZnO:12.8-14.2wt%;V2O5:3.8- 5.2wt%;MoO3:1.8-3.2wt%;TiO2: 0.8-1.2wt%; Residue is nickel powder; Auxiliary element and molar percentage are pressed oxygenCompound is calculated as: MnCO3:0.015-0.025wt%;CaCO3:0.03-0.04wt%;SiO2:0.04-0.05wt%;Al2O3: 0.02-0.04wt%;Bi2O3:0.008-0.012wt%;WO3:0.002-0.004wt%;Pr6O11:0.004-0.005wt%。
Preferably, by principal component and auxiliary element in molar ratio 1:0.35 make, wherein said principal component and quality hundredProportion by subtraction is calculated as by oxide: Fe2O3:53.55wt%;ZnO:13.5wt%;V2O5:4.5wt%;MoO3:2.5wt%;TiO2:1.0wt%; Residue is nickel powder; Auxiliary element and molar percentage are calculated as by oxide: MnCO3:0.02wt%;CaCO3: 0.035wt%;SiO2:0.045wt%;Al2O3:0.03wt%;Bi2O3:0.010wt%;WO3:0.003wt%;Pr6O11: 0.0045wt%。
The preparation method of a kind of soft magnetic ferrite with high initial permeability of the present invention, is characterized in that, bagDraw together following steps:
S1, mixing: by carrying out dry mixed after principal component proportion ingredient;
S2, pre-burning: the material mixing is carried out in pushed bat kiln to pre-burning;
S3, pulverizing: after adding auxiliary element in the principal component Preburning material obtaining in upper step pre-burning, carry out wet pulverizing;
S4, granulation: add the PVA of the 1.6-2.2% that is equivalent to slip weight at the slip of upper step, adopt mist projection granulating,Obtain particulate material;
S5, compacting: adopt powder former compacting to obtain blank the particulate material of upper step;
S6, sintering: in resistance furnace, carry out sintering, sintering temperature is controlled at 1100-1140 DEG C, insulation 240-300min,Sintering atmosphere is air, after sintering finishes, cools to room temperature with the furnace.
Preferably, in S1, incorporation time is 60-90min.
Preferably, in S2, calcined temperature control is 950-1250 DEG C, and the pre-burning time is 240-300min.
Preferably, in S3, grinding time is 60-100min, and after pulverizing, slip particle diameter is controlled at 1.6-2.0 μ m.
Preferably, in S5, the pressed density of blank is controlled at 3.15-3.45g/cm3
A kind of soft magnetic ferrite with high initial permeability of the present invention, presses certain by principal component and auxiliary elementRatio is made; Wherein said principal component comprises: Fe2O3、ZnO、V2O5、MoO3And TiO2, remain as nickel powder; Auxiliary element bagDraw together: MnCO3、CaCO3、SiO2、Al2O3、Bi2O3、WO3、Pr6O11. By Fe2O3、ZnO、V2O5、MoO3And TiO2Carry out dry mixedAfter carry out preheating, then add MnCO3、CaCO3、SiO2、Al2O3、Bi2O3、WO3And Pr6O11Carry out wet pulverizing, thenAdd PVA to carry out mist projection granulating, then make blank, then carry out sintering processes, finally obtain of the present invention have high initialThe soft magnetic ferrite of magnetic conductivity. Wherein, in principal component, both added TiO2Add again MoO3,TiO2Add can be obviousReduce iron loss, but can make magnetic conductivity reduce simultaneously, add appropriate MoO3Can this harmful effect of balance, reach optimum efficiency and makeThe initial permeability that obtains soft magnetic ferrite of the present invention has reached 6565.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail, should understands, embodiment is only for illustrating thisBright, instead of for the present invention is limited, any amendment of making, be equal to replacement etc. all at this on basis of the present inventionIn bright protection domain.
Embodiment 1
A kind of soft magnetic ferrite with high initial permeability that the present invention proposes, is pressed by principal component and auxiliary elementMol ratio 1:0.35 makes, and wherein said principal component and mass percent are calculated as by oxide: Fe2O3:53.55wt%; ZnO:13.5wt%;V2O5:4.5wt%;MoO3:2.5wt%;TiO2: 1.0wt%; Residue is nickel powder; Auxiliary element and molePercentage is calculated as by oxide: MnCO3:0.02wt%;CaCO3:0.035wt%;SiO2:0.045wt%;Al2O3: 0.03wt%;Bi2O3:0.010wt%;WO3:0.003wt%;Pr6O11:0.0045wt%。
Embodiment 2
A kind of soft magnetic ferrite with high initial permeability that the present invention proposes, is pressed by principal component and auxiliary elementMol ratio 1:0.3 makes, and wherein said principal component and mass percent are calculated as by oxide: Fe2O3:52.5wt%;ZnO: 14.5wt%;V2O5:3.5wt%;MoO3:3.5wt%;TiO2: 0.5wt%; Residue is nickel powder; Auxiliary element and mole percentageThan being calculated as by oxide: MnCO3:0.03wt%;CaCO3:0.02wt%;SiO2:0.06wt%;Al2O3:0.01wt%; Bi2O3:0.015wt%;WO3:0.001wt%;Pr6O11:0.006wt%。
The preparation method of a kind of soft magnetic ferrite with high initial permeability of the present invention, comprises the steps:
S1, mixing: by carrying out dry mixed after principal component proportion ingredient, incorporation time is 60min;
S2, pre-burning: the material mixing is carried out in pushed bat kiln to pre-burning, calcined temperature control is 1250 DEG C, when pre-burningBetween be 240min;
S3, pulverizing: after adding auxiliary element in the principal component Preburning material obtaining in upper step pre-burning, carry out wet pulverizing, pulverizeTime is 100min, and after pulverizing, slip particle diameter is controlled at 1.6 μ m;
S4, granulation: add 2.2% the PVA that is equivalent to slip weight at the slip of upper step, adopt mist projection granulating, obtainParticulate material;
S5, compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at 3.15g/cm3
S6, sintering: in resistance furnace, carry out sintering, sintering temperature is controlled at 1140 DEG C, insulation 240min, sintering atmosphere isAir, cools to room temperature with the furnace after sintering finishes.
Embodiment 3
A kind of soft magnetic ferrite with high initial permeability that the present invention proposes, is pressed by principal component and auxiliary elementMol ratio 1:0.4 makes, and wherein said principal component and mass percent are calculated as by oxide: Fe2O3:54.6wt%;ZnO: 12.5wt%;V2O5:5.5wt%;MoO3:1.5wt%;TiO2: 1.5wt%; Residue is nickel powder; Auxiliary element and mole percentageThan being calculated as by oxide: MnCO3:0.01wt%;CaCO3:0.05wt%;SiO2:0.03wt%;Al2O3:0.05wt%; Bi2O3:0.005wt%;WO3:0.005wt%;Pr6O11:0.003wt%。
The preparation method of a kind of soft magnetic ferrite with high initial permeability of the present invention, comprises the steps:
S1, mixing: by carrying out dry mixed after principal component proportion ingredient, incorporation time is 90min;
S2, pre-burning: the material mixing is carried out in pushed bat kiln to pre-burning, calcined temperature control is 950 DEG C, the pre-burning timeFor 300min;
S3, pulverizing: after adding auxiliary element in the principal component Preburning material obtaining in upper step pre-burning, carry out wet pulverizing, pulverizeTime is 60min, and after pulverizing, slip particle diameter is controlled at 2.0 μ m;
S4, granulation: add 1.6% the PVA that is equivalent to slip weight at the slip of upper step, adopt mist projection granulating, obtainParticulate material;
S5, compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at 3.45g/cm3
S6, sintering: in resistance furnace, carry out sintering, sintering temperature is controlled at 1100 DEG C, insulation 300min, sintering atmosphere isAir, cools to room temperature with the furnace after sintering finishes.
Embodiment 4
A kind of soft magnetic ferrite with high initial permeability that the present invention proposes, is pressed by principal component and auxiliary elementMol ratio 1:0.32 makes, and wherein said principal component and mass percent are calculated as by oxide: Fe2O3:52.8wt%; ZnO:14.2wt%;V2O5:3.8wt%;MoO3:3.2wt%;TiO2: 0.8wt%; Residue is nickel powder; Auxiliary element and molePercentage is calculated as by oxide: MnCO3:0.025wt%;CaCO3:0.03wt%;SiO2:0.05wt%;Al2O3: 0.02wt%;Bi2O3:0.012wt%;WO3:0.002wt%;Pr6O11:0.005wt%。
The preparation method of a kind of soft magnetic ferrite with high initial permeability of the present invention, comprises the steps:
S1, mixing: by carrying out dry mixed after principal component proportion ingredient, incorporation time is 65min;
S2, pre-burning: the material mixing is carried out in pushed bat kiln to pre-burning, calcined temperature control is 1220 DEG C, when pre-burningBetween be 250min;
S3, pulverizing: after adding auxiliary element in the principal component Preburning material obtaining in upper step pre-burning, carry out wet pulverizing, pulverizeTime is 90min, and after pulverizing, slip particle diameter is controlled at 1.7 μ m;
S4, granulation: add 2.1% the PVA that is equivalent to slip weight at the slip of upper step, adopt mist projection granulating, obtainParticulate material;
S5, compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at 3.25g/cm3
S6, sintering: in resistance furnace, carry out sintering, sintering temperature is controlled at 1130 DEG C, insulation 250min, sintering atmosphere isAir, cools to room temperature with the furnace after sintering finishes.
Embodiment 5
A kind of soft magnetic ferrite with high initial permeability that the present invention proposes, is pressed by principal component and auxiliary elementMol ratio 1:0.38 makes, and wherein said principal component and mass percent are calculated as by oxide: Fe2O3:54.3wt%; ZnO:12.8wt%;V2O5:5.2wt%;MoO3:1.8wt%;TiO2: 1.2wt%; Residue is nickel powder; Auxiliary element and molePercentage is calculated as by oxide: MnCO3:0.015wt%;CaCO3:0.04wt%;SiO2:0.04wt%;Al2O3: 0.04wt%;Bi2O3:0.008wt%;WO3:0.004wt%;Pr6O11:0.005wt%。
The preparation method of a kind of soft magnetic ferrite with high initial permeability of the present invention, comprises the steps:
S1, mixing: by carrying out dry mixed after principal component proportion ingredient, incorporation time is 85min;
S2, pre-burning: the material mixing is carried out in pushed bat kiln to pre-burning, calcined temperature control is 980 DEG C, the pre-burning timeFor 290min;
S3, pulverizing: after adding auxiliary element in the principal component Preburning material obtaining in upper step pre-burning, carry out wet pulverizing, pulverizeTime is 70min, and after pulverizing, slip particle diameter is controlled at 1.9 μ m;
S4, granulation: add 1.7% the PVA that is equivalent to slip weight at the slip of upper step, adopt mist projection granulating, obtainParticulate material;
S5, compacting: adopt powder former compacting to obtain blank the particulate material of upper step, the pressed density of blank is controlled at 3.35g/cm3
S6, sintering: in resistance furnace, carry out sintering, sintering temperature is controlled at 1110 DEG C, insulation 290min, sintering atmosphere isAir, cools to room temperature with the furnace after sintering finishes.
The soft magnetic ferrite with high initial permeability obtaining in embodiment 1-embodiment 5 is carried out to performance surveyExamination, the characteristic obtaining is as shown in table 1.
Table 1:
The above, be only preferably detailed description of the invention of the present invention, but protection scope of the present invention is not limited to this,Anyly be familiar with in technical scope that those skilled in the art disclose in the present invention, according to technical scheme of the present invention andInventive concept is equal to replaces or changes, within all should being encompassed in protection scope of the present invention.

Claims (10)

1. a soft magnetic ferrite with high initial permeability, is characterized in that, is massaged by principal component and auxiliary elementYou are than 1:(0.3-0.4) make;
Wherein said principal component and mass percent are calculated as by oxide:
Fe2O3:52.5-54.6wt%;
ZnO:12.5-14.5wt%;
V2O5:3.5-5.5wt%;
MoO3:1.5-3.5wt%;
TiO2:0.5-1.5wt%;
Residue is nickel powder;
Auxiliary element and molar percentage are calculated as by oxide:
MnCO3:0.01-0.03wt%;
CaCO3:0.02-0.05wt%;
SiO2:0.03-0.06wt%;
Al2O3:0.01-0.05wt%;
Bi2O3:0.005-0.015wt%;
WO3:0.001-0.005wt%;
Pr6O11:0.003-0.006wt%。
2. the soft magnetic ferrite with high initial permeability according to claim 1, is characterized in that principal componentIn, Fe2O3、ZnO、V2O5、MoO3And TiO2Mass percent be 52.8-54.3:12.8-14.2:3.8-5.2:1.8-3.2: 0.8-1.2。
3. the soft magnetic ferrite with high initial permeability according to claim 1 and 2, is characterized in that, auxiliaryIn composition, MnCO3、CaCO3、SiO2、Al2O3、Bi2O3、WO3And Pr6O11Mass percent be 0.015-0.025:0.03- 0.04:0.04-0.05:0.02-0.04:0.008-0.012:0.002-0.004:0.004-0.005。
4. according to the soft magnetic ferrite with high initial permeability described in claim 1-3 any one, it is characterized in that,By principal component and auxiliary element 1:(0.32-0.38 in molar ratio) to make, wherein said principal component and mass percent are pressed oxygenCompound is calculated as: Fe2O3:52.8-54.3wt%;ZnO:12.8-14.2wt%;V2O5:3.8-5.2wt%;MoO3:1.8- 3.2wt%;TiO2: 0.8-1.2wt%; Residue is nickel powder; Auxiliary element and molar percentage are calculated as by oxide: MnCO3: 0.015-0.025wt%;CaCO3:0.03-0.04wt%;SiO2:0.04-0.05wt%;Al2O3:0.02-0.04wt%; Bi2O3:0.008-0.012wt%;WO3:0.002-0.004wt%;Pr6O11:0.004-0.005wt%。
5. according to the soft magnetic ferrite with high initial permeability described in claim 1-4 any one, it is characterized in that,By principal component and auxiliary element in molar ratio 1:0.35 make, wherein said principal component and mass percent are pressed oxide and are calculatedFor: Fe2O3:53.55wt%;ZnO:13.5wt%;V2O5:4.5wt%;MoO3:2.5wt%;TiO2: 1.0wt%; Residue is nickelPowder; Auxiliary element and molar percentage are calculated as by oxide: MnCO3:0.02wt%;CaCO3:0.035wt%;SiO2: 0.045wt%;Al2O3:0.03wt%;Bi2O3:0.010wt%;WO3:0.003wt%;Pr6O11:0.0045wt%。
6. one kind according to the preparation side of the soft magnetic ferrite with high initial permeability described in claim 1-5 any oneMethod, is characterized in that, comprises the steps:
S1, mixing: by carrying out dry mixed after principal component proportion ingredient;
S2, pre-burning: the material mixing is carried out in pushed bat kiln to pre-burning;
S3, pulverizing: after adding auxiliary element in the principal component Preburning material obtaining in upper step pre-burning, carry out wet pulverizing;
S4, granulation: add the PVA of the 1.6-2.2% that is equivalent to slip weight at the slip of upper step, adopt mist projection granulating, obtainParticulate material;
S5, compacting: adopt powder former compacting to obtain blank the particulate material of upper step;
S6, sintering: in resistance furnace, carry out sintering, sintering temperature is controlled at 1100-1140 DEG C, insulation 240-300min, sinteringAtmosphere is air, after sintering finishes, cools to room temperature with the furnace.
7. the preparation method of the soft magnetic ferrite with high initial permeability according to claim 6, its feature existsIn, in S1, incorporation time is 60-90min.
8. according to the preparation method of the soft magnetic ferrite with high initial permeability described in claim 6 or 7, its featureBe, in S2, calcined temperature control is 950-1250 DEG C, and the pre-burning time is 240-300min.
9. according to the preparation method of the soft magnetic ferrite with high initial permeability described in claim 6-8 any one,It is characterized in that, in S3, grinding time is 60-100min, and after pulverizing, slip particle diameter is controlled at 1.6-2.0 μ m.
10. according to the preparation method of the soft magnetic ferrite with high initial permeability described in claim 6-9 any one,It is characterized in that, in S5, the pressed density of blank is controlled at 3.15-3.45g/cm3
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