CN109553408A - A kind of preparation method of rear-earth-doped MnZn ferrite material - Google Patents
A kind of preparation method of rear-earth-doped MnZn ferrite material Download PDFInfo
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Abstract
The present invention relates to technical field of magnetic materials, the invention discloses a kind of preparation method of rear-earth-doped MnZn ferrite material, include the following steps: principal component manganese oxide, zinc oxide, iron oxide ball mill ball milling is added, obtain mixture A；Mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；Ball mill secondary ball milling is added in Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, combined rare earth additive, drying obtains mixture B；The combined rare earth additive is made of cerium sesquioxide, yttrium oxide, lanthana；Poly-vinyl alcohol solution mixing granulation is added into mixture B, then crosses 40-80 mesh, obtains particulate material；Particulate material is added in molding machine and is suppressed, blank is obtained；It is sintered blank, after cooling.Rear-earth-doped MnZn ferrite material prepared by the present invention initial permeability with higher and saturation flux density.
Description
Technical field
The present invention relates to technical field of magnetic materials more particularly to a kind of preparation sides of rear-earth-doped MnZn ferrite material
Method.
Background technique
The application of soft magnetic materials in the industry starts from late nineteenth century, is the rise along with electric power electrician and telecom technology
And occur, application range is extremely extensive.Soft magnetic materials be not only applicable to field of household appliances, informatization, automotive field and
Other mating fields, the main raw material(s) more important is soft magnetic materials as Electronic Components Manufacturing are brought in a steady stream not for it
Disconnected demand.And with the extension of the development of electronics industry and application field, the requirement to magnetic material is also higher and higher.It is existing
The magnetic conductivity of soft magnetic ferrite in technology is unable to satisfy the demand of the prior art, therefore needs to design a kind of high magnetic permeability soft magnetism
Ferrite Material solves the problems of the prior art.
Summary of the invention
Based on background technique there are the problem of, the invention proposes a kind of preparation sides of rear-earth-doped MnZn ferrite material
Method, rear-earth-doped MnZn ferrite material prepared by the present invention initial permeability with higher and saturation flux density.
The invention proposes a kind of preparation methods of rear-earth-doped MnZn ferrite material, include the following steps:
S1, ball mill ball milling is added in principal component manganese oxide, zinc oxide, iron oxide, obtains mixture A；Wherein manganese oxide,
Zinc oxide, iron oxide molar ratio be 35-37:53-55:9-11；
S2, mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；
S3, by Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, compound dilute
Ball mill secondary ball milling is added in soil additive, and drying obtains mixture B；The combined rare earth additive be by cerium sesquioxide,
Yttrium oxide, lanthana composition；
S4, poly-vinyl alcohol solution mixing granulation is added into mixture B, then crosses 40-80 mesh, obtains particulate material；It is mixed
The mass ratio for closing material B and poly-vinyl alcohol solution is 80-90:10-12；
S5, particulate material is added in molding machine and is suppressed, obtain blank；
S6, by blank 1350-1380 DEG C at a temperature of be sintered and cooled after.
Preferably, in S1, drum's speed of rotation 150-200r/min, Ball-milling Time 4-6h.
Preferably, in S2, calcined temperature is 860-880 DEG C, burn-in time 60-90min.
Preferably, in S3, Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide,
The mass ratio of combined rare earth additive is 9800-10000:2-3:1-2:1-2:1.5-3:1.5-2.5:0.5-1.5:6-10.
Preferably, in S3, the combined rare earth additive is by cerium sesquioxide, yttrium oxide, lanthana 3- in mass ratio
4:4-5:6-8 composition.
Preferably, in S3, drum's speed of rotation 150-200r/min, Ball-milling Time 2-3h.
Preferably, in S4, using mass fraction is the poly-vinyl alcohol solution of 8-10%.
Preferably, in S6, soaking time 4-5h.
In the present invention, the addition of vanadium oxide helps to form liquid phase during the sintering process, increases liquid-solid reaction area, makes anti-
It answers rate to accelerate, and manganese-zinc ferrite crystal grain is made uniformly to grow up, to increase the magnetic conductivity and saturation induction of manganese-zinc ferrite
Intensity；The addition of niobium pentaoxide can refine crystal grain, make manganese-zinc ferrite crystal grain even compact, can also prevent waving for zinc
Hair, and then improve manganese-zinc ferrite initial permeability and reduce loss；Suitable bismuth oxide is added and is conducive to manganese-zinc ferrite crystalline substance
Uniformly growing up for grain, reduces the porosity, increases density, final to improve manganese-zinc ferrite initial permeability；Add suitable oxidation
Molybdenum can refine manganese-zinc ferrite crystal grain, play the role of the sintered density and initial permeability that improve manganese-zinc ferrite；It is added
Phosphorus pentoxide can increase the vacancy of metal ion near crystal boundary, accelerate the movement of crystal boundary, and increase manganese-zinc ferrite crystal grain
Size and density, and then play the role of enhancing manganese-zinc ferrite initial permeability；Copper oxide can reduce sintering temperature, increase
Lattice constant promotes crystal grain to grow up, and the appropriate copper oxide that is added can reduce the porosity of manganese-zinc ferrite and improve its resistivity
And initial permeability；With the addition of lanthana, Ln3+It is a small amount of to replace Fe3+Afterwards, the superexchange being more advantageous between metal ion
Effect, to improve ferritic initial permeability and saturation magnetic conductivity；Cerium sesquioxide, which is added, can be improved the burning of sample
Density is tied, stomata quantity is reduced, and then improves ferritic initial permeability and saturation magnetic conductivity；Suitable yttrium oxide is added
Can reduce the stomata quantity of sample, the solid phase reaction during acceleration of sintering, play improve ferritic initial permeability with
And the effect of saturation magnetic conductivity.Why calcined temperature is limited to 860-880 DEG C by the present invention in a preferred approach, is because closing
The calcined temperature of reason can optimize the physical and chemical properties of particulate material, obtain better shaping density and sintered density, reduction
The porosity uniformly refines crystal grain, to reduce the magnetic conductivity that loss improves MnZn ferrite material.
The present invention significantly changes MnZn ferrite material crystal grain by way of adding suitable compound additive
Crystal boundary composition, ionic valence condition and microstructure, in conjunction with reasonable preparation process, and then make MnZn ferrite material obtained
Initial permeability and saturation flux density etc..
Specific embodiment
Technical solution of the present invention is described in detail combined with specific embodiments below.
Embodiment 1
A kind of preparation method of rear-earth-doped MnZn ferrite material, includes the following steps:
S1, ball mill ball milling is added in principal component manganese oxide, zinc oxide, iron oxide, obtains mixture A；Wherein manganese oxide,
Zinc oxide, iron oxide molar ratio be 35:55:9；
S2, mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；
S3, by Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, compound dilute
Ball mill secondary ball milling is added in soil additive, and drying obtains mixture B；The combined rare earth additive be by cerium sesquioxide,
Yttrium oxide, lanthana composition；
S4, poly-vinyl alcohol solution mixing granulation is added into mixture B, then crosses 40 meshes, obtains particulate material；Mixture
The mass ratio of B and poly-vinyl alcohol solution is 90:10；
S5, particulate material is added in molding machine and is suppressed, obtain blank；
S6, by blank 1350 DEG C at a temperature of be sintered and cooled after.
Embodiment 2
A kind of preparation method of rear-earth-doped MnZn ferrite material, includes the following steps:
S1, ball mill ball milling is added in principal component manganese oxide, zinc oxide, iron oxide, obtains mixture A；Wherein manganese oxide,
Zinc oxide, iron oxide molar ratio be 37:53:11；
S2, mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；
S3, by Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, compound dilute
Ball mill secondary ball milling is added in soil additive, and drying obtains mixture B；The combined rare earth additive be by cerium sesquioxide,
Yttrium oxide, lanthana composition；
S4, poly-vinyl alcohol solution mixing granulation is added into mixture B, then crosses 80 meshes, obtains particulate material；Mixture
The mass ratio of B and poly-vinyl alcohol solution is 80:12；
S5, particulate material is added in molding machine and is suppressed, obtain blank；
S6, by blank 1380 DEG C at a temperature of be sintered and cooled after.
Embodiment 3
A kind of preparation method of rear-earth-doped MnZn ferrite material, includes the following steps:
S1, ball mill ball milling is added in principal component manganese oxide, zinc oxide, iron oxide, obtains mixture A；Wherein manganese oxide,
Zinc oxide, iron oxide molar ratio be 35:55:9；Drum's speed of rotation is 150r/min, Ball-milling Time 6h；
S2, mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；Calcined temperature is 860 DEG C, when pre-burning
Between be 90min；
S3, by Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, compound dilute
Ball mill secondary ball milling is added in soil additive, and drying obtains mixture B；Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide,
Molybdenum oxide, phosphorus pentoxide, copper oxide, combined rare earth additive mass ratio be 9800:3:1:2:1.5:2.5:0.5:10；Institute
Combined rare earth additive is stated to be made of cerium sesquioxide, yttrium oxide, lanthana 3:5:6 in mass ratio；Drum's speed of rotation is
150r/min, Ball-milling Time 3h；
S4, the poly-vinyl alcohol solution mixing granulation that mass fraction is 8% is added into mixture B, then crosses 40 meshes, obtains
To particulate material；The mass ratio of mixture B and poly-vinyl alcohol solution is 90:10；
S5, particulate material is added in molding machine and is suppressed, obtain blank；
S6, by blank 1350 DEG C at a temperature of be sintered, soaking time 4h, after cooling.
Embodiment 4
A kind of preparation method of rear-earth-doped MnZn ferrite material, includes the following steps:
S1, ball mill ball milling is added in principal component manganese oxide, zinc oxide, iron oxide, obtains mixture A；Wherein manganese oxide,
Zinc oxide, iron oxide molar ratio be 37:53:11；Drum's speed of rotation is 200r/min, Ball-milling Time 4h；
S2, mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；Calcined temperature is 880 DEG C, when pre-burning
Between be 60min；
S3, by Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, compound dilute
Ball mill secondary ball milling is added in soil additive, and drying obtains mixture B；Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide,
Molybdenum oxide, phosphorus pentoxide, copper oxide, combined rare earth additive mass ratio be 10000:2:2:1:3:1.5:1.5:6；It is described
Combined rare earth additive is made of cerium sesquioxide, yttrium oxide, lanthana 4:4:8 in mass ratio；Drum's speed of rotation is 200r/
Min, Ball-milling Time 2h；
S4, the poly-vinyl alcohol solution mixing granulation that mass fraction is 10% is added into mixture B, then crosses 80 meshes,
Obtain particulate material；The mass ratio of mixture B and poly-vinyl alcohol solution is 80:12；
S5, particulate material is added in molding machine and is suppressed, obtain blank；
S6, by blank 1380 DEG C at a temperature of be sintered, soaking time 5h, after cooling.
Experimental example
The initial permeability and saturation flux density of the rear-earth-doped MnZn ferrite material of embodiment 1-4 preparation are detected,
Experimental result is as shown in table 1:
Table 1
As shown in Table 1, rear-earth-doped MnZn ferrite material initial permeability with higher prepared by the present invention and full
And magnetic flux density.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of rear-earth-doped MnZn ferrite material, which comprises the steps of:
S1, ball mill ball milling is added in principal component manganese oxide, zinc oxide, iron oxide, obtains mixture A；Wherein manganese oxide, oxidation
Zinc, iron oxide molar ratio be 35-37:53-55:9-11；
S2, mixture A is subjected to pre-burning, then cools to room temperature, obtains Preburning material；
S3, Preburning material, vanadium oxide, niobium pentaoxide, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, compound rare-earth are added
Add agent that ball mill secondary ball milling is added, drying obtains mixture B；The combined rare earth additive is by cerium sesquioxide, oxidation
Yttrium, lanthana composition；
S4, poly-vinyl alcohol solution mixing granulation is added into mixture B, then crosses 40-80 mesh, obtains particulate material；Mixture B
Mass ratio with poly-vinyl alcohol solution is 80-90:10-12；
S5, particulate material is added in molding machine and is suppressed, obtain blank；
S6, by blank 1350-1380 DEG C at a temperature of be sintered and cooled after.
2. preparation method according to claim 1, which is characterized in that in S1, drum's speed of rotation 150-200r/min, ball
Time consuming is 4-6h.
3. preparation method according to claim 1 or 2, which is characterized in that in S2, calcined temperature is 860-880 DEG C, pre-burning
Time is 60-90min.
4. preparation method according to claim 1-3, which is characterized in that in S3, Preburning material, vanadium oxide, five oxygen
Change two niobiums, bismuth oxide, molybdenum oxide, phosphorus pentoxide, copper oxide, combined rare earth additive mass ratio be 9800-10000:2-
3:1-2:1-2:1.5-3:1.5-2.5:0.5-1.5:6-10。
5. preparation method according to claim 1-4, which is characterized in that in S3, the combined rare earth additive
It is made of cerium sesquioxide, yttrium oxide, lanthana 3-4:4-5:6-8 in mass ratio.
6. preparation method according to claim 1-5, which is characterized in that in S3, drum's speed of rotation 150-
200r/min, Ball-milling Time 2-3h.
7. preparation method according to claim 1-6, which is characterized in that in S4, use the mass fraction to be
The poly-vinyl alcohol solution of 8-10%.
8. preparation method according to claim 1-7, which is characterized in that in S6, soaking time 4-5h.
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| CN111517776A (en) * | 2020-04-23 | 2020-08-11 | 眉山市宇泰电子设备有限公司 | Preparation method of manganese-zinc soft magnetic ferrite material |
| CN111825440A (en) * | 2019-04-19 | 2020-10-27 | 佛山市顺德区美的电热电器制造有限公司 | Manganese-zinc ferrite and preparation method and application thereof |
| CN111825439A (en) * | 2019-04-19 | 2020-10-27 | 佛山市顺德区美的电热电器制造有限公司 | Manganese-zinc ferrite and preparation method and application thereof |
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