CN114804849B - Nickel-zinc ferrite magnetic core and preparation method and application thereof - Google Patents

Nickel-zinc ferrite magnetic core and preparation method and application thereof Download PDF

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CN114804849B
CN114804849B CN202210547181.4A CN202210547181A CN114804849B CN 114804849 B CN114804849 B CN 114804849B CN 202210547181 A CN202210547181 A CN 202210547181A CN 114804849 B CN114804849 B CN 114804849B
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蒋仲翔
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Guangdong Fanrui New Material Co ltd
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Abstract

The invention discloses a nickel-zinc ferrite magnetic core and a preparation method and application thereof. The preparation method of the nickel-zinc ferrite magnetic core comprises the following steps: 1) Mixing Fe 2 O 3 Mixing the powder, znO powder and NiO powder to prepare magnetic powder; 2) Mixing magnetic powder, polyvinyl alcohol and silica sol, and pressing into a prefabricated blank; 3) Pre-burning the prefabricated blank body, and then crushing the prefabricated blank body to prepare pre-burned magnetic powder; 4) Pre-burning magnetic powder and SiO 2 ‑B 2 O 3 ‑Al 2 O 3 Mixing the glass powder and then ball-milling to prepare blended powder; 5) Mixing the blending powder, carbonate, polyvinyl alcohol and a coupling agent, and then granulating to obtain granules; 6) And injecting the granules into a mold to be pressed into a magnetic core blank, and sintering. The nickel-zinc ferrite magnetic core has the advantages of high inductance value, high strength, simple preparation process and low cost, can meet the application requirements of high frequency and large working current, and has wide application prospect.

Description

Nickel-zinc ferrite magnetic core and preparation method and application thereof
Technical Field
The invention relates to the technical field of soft magnetic ferrite, in particular to a nickel-zinc ferrite magnetic core and a preparation method and application thereof.
Background
As the inductance element is developed to have a higher frequency and a lower loss, its size becomes smaller, and its operating current becomes larger as the power increases. Although the magnetic core made of the existing soft magnetic alloy material can be applied to scenes with large working current and frequency not more than 10MHz, the magnetic core has the problems of poor insulation and unstable high frequency, and cannot be applied to scenes with frequency more than 10 MHz. The magnetic core insulating nature that ferrite material made is good, high frequency stable performance, can use the scene more than frequency 10MHz, but along with the increase of operating current, in order to reduce and generate heat, need increase the line footpath of copper line, this just leads to needing bigger wire winding tension can be flat ground and wind the coil on the magnetic core, and the intensity of current ferrite magnetic core can't satisfy the coiling requirement of big line footpath copper line at all, serious damage can appear in the magnetic core during wire winding preparation coil, the product yield is low.
Therefore, it is highly desirable to develop a nickel-zinc-ferrite core having a high strength while maintaining a high inductance value.
The foregoing merely provides background information related to the present invention and does not necessarily constitute prior art.
Disclosure of Invention
An object of the present invention is to provide a nickel-zinc-ferrite core having both a high inductance value and a high strength.
The second purpose of the invention is to provide a preparation method of the nickel-zinc ferrite magnetic core.
The invention also aims to provide an inductor comprising the nickel-zinc ferrite magnetic core.
The technical scheme adopted by the invention is as follows:
a preparation method of a nickel-zinc ferrite magnetic core comprises the following steps:
1) Mixing Fe 2 O 3 Mixing the powder, znO powder and NiO powder to obtain magnetic powder;
2) Mixing magnetic powder, polyvinyl alcohol and silica sol, and pressing to obtain a prefabricated blank;
3) Pre-burning the prefabricated blank body and then crushing to obtain pre-burned magnetic powder;
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Mixing the glass powder and then performing ball milling to obtain blended powder;
5) Mixing the blended powder, carbonate, polyvinyl alcohol and a coupling agent, and then granulating to obtain granules;
6) And injecting the particles into a mold to be pressed into a magnetic core blank, and sintering to obtain the nickel-zinc ferrite magnetic core.
Preferably, the magnetic powder in step 1) comprises the following components in percentage by mass:
Fe 2 O 3 powder: 62 to 72 percent;
ZnO powder: 10% -13%;
NiO powder: 18 to 25 percent.
Preferably, said Fe of step 1) 2 O 3 The powder has an average particle diameter of 0.8 to 1.5 μm.
Preferably, the polyvinyl alcohol in the step 2) is added in an amount of 1.0 to 3.0% by mass based on the magnetic powder.
Preferably, the mass ratio of the polyvinyl alcohol to the silica sol in the step 2) is 1 to 4.
Preferably, the polyvinyl alcohol in the step 2) has the number average molecular weight of 130000g/mol to 210000g/mol.
Preferably, the density of the precast blank body of the step 2) is 2.5g/cm 3 ~2.8g/cm 3
Preferably, the pre-sintering in the step 3) is carried out in an air atmosphere, the pre-sintering temperature is 950-1100 ℃, and the pre-sintering time is 2-4 hours.
Preferably, the particle size of the calcined magnetic powder in step 3) is 1 to 5 μm.
Preferably, step 4) said SiO 2 -B 2 O 3 -Al 2 O 3 The adding amount of the glass powder is 0.1-1.0% of the mass of the pre-sintered magnetic powder.
Preferably, step 4) said SiO 2 -B 2 O 3 -Al 2 O 3 The glass powder comprises the following components in percentage by mass:
SiO 2 :50%~65%;
B 2 O 3 :10%~15%;
Al 2 O 3 :25%~35%。
preferably, step 4) is performed using SiO 2 -B 2 O 3 -Al 2 O 3 The average grain diameter of the glass powder is 0.8-2.0 μm.
Preferably, the addition amount of the carbonate in the step 5) is 0.01-0.50% of the mass of the blended powder.
Preferably, the carbonate in step 5) is at least one of lithium carbonate and manganese carbonate.
Preferably, the carbonate in step 5) has an average particle size of 0.3 to 1.0. Mu.m.
Preferably, the addition amount of the polyvinyl alcohol in the step 5) is 1.0-3.0% of the total mass of the blending powder and the carbonate.
Preferably, the polyvinyl alcohol in the step 5) has the number average molecular weight of 130000g/mol to 210000g/mol.
Preferably, the addition amount of the coupling agent in the step 5) is 0.01-0.10% of the total mass of the blending powder and the carbonate.
Preferably, the coupling agent in the step 5) is at least one of long-chain methoxy silane and long-chain ethoxy silane.
Preferably, the sintering in the step 6) is carried out in an air atmosphere, the sintering temperature is 1100-1200 ℃, and the sintering time is 1-3 h.
A nickel-zinc ferrite core is prepared by the preparation method.
An inductance component comprises the nickel-zinc-ferrite core.
The invention has the beneficial effects that: the nickel-zinc ferrite magnetic core has the advantages of high inductance value, high strength, simple preparation process and low cost, can meet the application requirements of high frequency and large working current, and has wide application prospect.
Specifically, the method comprises the following steps: the invention mixes and presses the magnetic powder, the polyvinyl alcohol and the silica sol into a prefabricated blank body, then presintering and crushing are carried out, the generation of a nickel-zinc ferrite spinel phase can be promoted, and SiO-containing particles can be formed firstly 2 Keeping the magnetic conductivity and saturation performance of the material, and then adding SiO into the preburning magnetic powder which already forms spinel phase 2 -B 2 O 3 -Al 2 O 3 Sintering the glass powder, the carbonate, the polyvinyl alcohol and the coupling agent to form a composite film layer of glass and the auxiliary agent, and further mixing the composite film layer with the SiO formed in the initial stage 2 The composite grain boundary is formed by the grain boundary structure, and the finally obtained nickel-zinc ferrite magnetic core has extremely high density and high strength, so that the magnetic core can be prevented from being damaged under large winding stress.
Drawings
Fig. 1 is a schematic view of the structures of nickel-zinc-ferrite cores of examples 1 to 3 and comparative examples 1 to 3.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a nickel-zinc-ferrite core (the schematic structural diagram is shown in figure 1, a is a cross section, b is a top surface) is prepared by the following steps:
1) Mixing Fe 2 O 3 Uniformly mixing powder (with an average particle size of 0.8 μm), znO powder and NiO powder according to a mass ratio of 72;
2) Uniformly mixing magnetic powder, polyvinyl alcohol (with the number average molecular weight of 210000 g/mol) and silica sol, wherein the addition amount of the polyvinyl alcohol is 1.0% of the mass of the magnetic powder, the mass ratio of the polyvinyl alcohol to the silica sol is 4 3 );
3) Pre-sintering the prefabricated blank body in air atmosphere at 950 ℃ for 4h, and crushing after pre-sintering to obtain pre-sintered magnetic powder (the particle size is 1-5 mu m);
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Glass powder (average particle size of 2.0 μm) was mixed and ball-milled, siO 2 -B 2 O 3 -Al 2 O 3 The addition amount of the glass powder was 1.0% by mass of the calcined magnetic powder, and SiO was added 2 -B 2 O 3 -Al 2 O 3 The glass powder is made of SiO 2 、B 2 O 3 And Al 2 O 3 The powder mixture is composed of the following components in a mass ratio of 65;
5) Uniformly mixing the blended powder, manganese carbonate (with the average particle size of 1.0 mu m), polyvinyl alcohol (with the number average molecular weight of 210000 g/mol) and dodecyl methyl dimethoxy silane, wherein the addition amount of the manganese carbonate is 0.5 percent of the mass of the blended powder, the addition amount of the polyvinyl alcohol is 1.0 percent of the total mass of the blended powder and the manganese carbonate, and the addition amount of the dodecyl methyl dimethoxy silane is 0.01 percent of the total mass of the blended powder and the manganese carbonate, and then granulating to obtain granules;
6) And injecting the particles into a mold to be pressed into a magnetic core blank, and sintering for 3 hours at 1100 ℃ in an air atmosphere to obtain the nickel-zinc ferrite magnetic core (size specification: the length of the blade is 2.5mm, the width of the blade is 2.0mm, the thickness of the blade is 0.28mm, and the diameter of the center pillar is 1.65 mm).
Example 2:
a nickel-zinc-ferrite core (the schematic structural diagram is shown in FIG. 1, a is a cross section, b is a top surface) is prepared by the following steps:
1) Mixing Fe 2 O 3 Uniformly mixing powder (average particle size of 1.5 μm), znO powder and NiO powder in a mass ratio of 62;
2) Uniformly mixing magnetic powder, polyvinyl alcohol (with the number average molecular weight of 130000 g/mol) and silica sol, wherein the addition amount of the polyvinyl alcohol is 3.0% of the mass of the magnetic powder, the mass ratio of the polyvinyl alcohol to the silica sol is 1, and then pressing to obtain a prefabricated blank (with the density of 2.5g/cm 3 );
3) Pre-sintering the prefabricated blank body in an air atmosphere at 1100 ℃ for 2h, and crushing the pre-sintered blank body after pre-sintering to obtain pre-sintered magnetic powder (the particle size is 1-5 mu m);
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Glass powder (average particle size of 0.8 μm) was mixed and ball-milled, siO 2 -B 2 O 3 -Al 2 O 3 The addition amount of the glass powder was 0.1% by mass of the pre-fired magnetic powder, and SiO 2 -B 2 O 3 -Al 2 O 3 The glass powder is made of SiO 2 、B 2 O 3 And Al 2 O 3 The powder is prepared from the following components in a mass ratio of 50;
5) Uniformly mixing the blended powder, lithium carbonate (the average particle size is 0.3 mu m), polyvinyl alcohol (the number average molecular weight is 130000 g/mol) and methyl propyl diethoxy silane, wherein the addition amount of the lithium carbonate is 0.01 percent of the mass of the blended powder, the addition amount of the polyvinyl alcohol is 3.0 percent of the total mass of the blended powder and the lithium carbonate, and the addition amount of the methyl propyl diethoxy silane is 0.1 percent of the total mass of the blended powder and the lithium carbonate, and then granulating to obtain a granular material;
6) And injecting the granules into a mold to be pressed into a magnetic core blank, and then sintering the magnetic core blank for 1h at 1200 ℃ in an air atmosphere to obtain the nickel-zinc ferrite magnetic core (the size and specification are the same as those of the embodiment 1).
Example 3:
a nickel-zinc-ferrite core (the schematic structural diagram is shown in figure 1, a is a cross section, b is a top surface) is prepared by the following steps:
1) Mixing Fe 2 O 3 Uniformly mixing powder (with an average particle size of 1.2 μm), znO powder and NiO powder according to a mass ratio of 67;
2) Uniformly mixing magnetic powder, polyvinyl alcohol (with the number average molecular weight of 170000 g/mol) and silica sol, wherein the addition amount of the polyvinyl alcohol is 2.0% of the mass of the magnetic powder, and the mass ratio of the polyvinyl alcohol to the silica sol is 3 3 );
3) Pre-sintering the prefabricated blank body in air atmosphere at 1050 ℃ for 3h, and crushing after pre-sintering to obtain pre-sintered magnetic powder (the particle size is 1-5 mu m);
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Glass powder (average particle size of 1.3 μm) was mixed and ball-milled, siO 2 -B 2 O 3 -Al 2 O 3 The addition amount of the glass powder was 0.5% by mass of the pre-fired magnetic powder, and SiO 2 -B 2 O 3 -Al 2 O 3 The glass powder is made of SiO 2 、B 2 O 3 And Al 2 O 3 The preparation method comprises the following steps of (1) obtaining blended powder according to the mass ratio of 60;
5) Uniformly mixing the blended powder, lithium carbonate (the average particle size is 0.8 mu m), polyvinyl alcohol (the number average molecular weight is 170000 g/mol) and dodecyl trimethoxy silane, wherein the addition amount of the lithium carbonate is 0.25 percent of the mass of the blended powder, the addition amount of the polyvinyl alcohol is 2.0 percent of the total mass of the blended powder and the lithium carbonate, and the addition amount of the dodecyl trimethoxy silane is 0.05 percent of the total mass of the blended powder and the lithium carbonate, and then granulating to obtain a granular material;
6) Injecting the granules into a mold to be pressed into a magnetic core blank, and then placing the magnetic core blank in an air atmosphere at 1160 ℃ for sintering for 2h to obtain the nickel-zinc ferrite magnetic core (the size and specification are the same as those of the example 1).
Comparative example 1:
a nickel-zinc-ferrite core (the schematic structural diagram is shown in FIG. 1, a is a cross section, b is a top surface) is prepared by the following steps:
1) Mixing Fe 2 O 3 Uniformly mixing powder (with the average particle size of 0.8 mu m), znO powder and NiO powder according to a mass ratio of 72;
2) Pre-sintered magnetic powder and Bi 2 O 3 Mixing the powders and ball milling to obtain Bi 2 O 3 The addition amount of the powder is 0.3% of the mass of the pre-sintered magnetic powder, so as to obtain blended powder;
3) And (3) uniformly mixing the blended powder and polyvinyl alcohol (the number average molecular weight is 210000 g/mol), wherein the addition amount of the polyvinyl alcohol is 1.5 percent of the mass of the blended powder, injecting the mixture into a mold to press the mixture into a magnetic core blank, and sintering the magnetic core blank in an air atmosphere at 1200 ℃ for 3 hours to obtain the nickel-zinc ferrite magnetic core (the size and the specification are the same as those of the example 1).
Comparative example 2:
a nickel-zinc-ferrite core (the schematic structural diagram is shown in FIG. 1, a is a cross section, b is a top surface) is prepared by the following steps:
1) Mixing Fe 2 O 3 Uniformly mixing powder (with an average particle size of 0.8 μm), znO powder and NiO powder according to a mass ratio of 72;
2) Uniformly mixing magnetic powder, polyvinyl alcohol (with the number average molecular weight of 130000 g/mol) and silica sol, wherein the addition amount of the polyvinyl alcohol is 1.0% of the mass of the magnetic powder, the mass ratio of the polyvinyl alcohol to the silica sol is 4 3 );
3) Pre-sintering the prefabricated blank body in air atmosphere at 950 ℃ for 4h, and crushing after pre-sintering to obtain pre-sintered magnetic powder (the particle size is 1-5 mu m);
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Mixing glass powder (average particle size of 2.0 μm), ball milling, and SiO 2 -B 2 O 3 -Al 2 O 3 The addition amount of the glass powder was 1.0% by mass of the calcined magnetic powder, and SiO 2 -B 2 O 3 -Al 2 O 3 The glass powder is made of SiO 2 、B 2 O 3 And Al 2 O 3 The preparation method comprises the following steps of (1) obtaining blended powder according to the mass ratio of 65;
5) Uniformly mixing the blended powder and polyvinyl alcohol (the number average molecular weight is 130000 g/mol), wherein the addition amount of the polyvinyl alcohol is 1.0 percent of the mass of the blended powder, and then granulating to obtain granules;
6) Injecting the granules into a mold to be pressed into a magnetic core blank, and then sintering the magnetic core blank for 3 hours at 1100 ℃ in an air atmosphere to obtain the nickel-zinc ferrite magnetic core (the size and specification are the same as those of the embodiment 1).
Comparative example 3:
a nickel-zinc-ferrite core (the schematic structural diagram is shown in figure 1, a is a cross section, b is a top surface) is prepared by the following steps:
1) Mixing Fe 2 O 3 Uniformly mixing powder (average particle size of 1.5 μm), znO powder and NiO powder in a mass ratio of 62;
2) Uniformly mixing magnetic powder, polyvinyl alcohol (with the number average molecular weight of 170000 g/mol) and silica sol, wherein the addition amount of the polyvinyl alcohol is 3.0% of the mass of the magnetic powder, and the mass ratio of the polyvinyl alcohol to the silica sol is 1, and then pressing to obtain a prefabricated blank (with the density of 2.5g/cm 3 );
3) Presintering the prefabricated blank body in an air atmosphere at 1100 ℃ for 2h, and then crushing to obtain presintered magnetic powder (the average particle size is 10 mu m);
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Glass powder (average particle size 5.0 μm) was mixed and ball-milled, siO 2 -B 2 O 3 -Al 2 O 3 The addition amount of the glass powder was 0.1% by mass of the calcined magnetic powder, and SiO was added 2 -B 2 O 3 -Al 2 O 3 The glass powder is made of SiO 2 、B 2 O 3 And Al 2 O 3 The powder comprises the following components in a mass ratio of 50;
5) Uniformly mixing the blended powder, lithium carbonate (the average particle size is 0.3 mu m), polyvinyl alcohol (the number average molecular weight is 170000 g/mol) and dodecyl trimethoxy silane, wherein the addition amount of the lithium carbonate is 0.25 percent of the mass of the blended powder, the addition amount of the polyvinyl alcohol is 3.0 percent of the total mass of the blended powder and the lithium carbonate, and the addition amount of the dodecyl trimethoxy silane is 0.1 percent of the total mass of the blended powder and the lithium carbonate, and then granulating to obtain a granular material;
6) And injecting the granules into a mold to be pressed into a magnetic core blank, and then sintering the magnetic core blank for 1h at 1200 ℃ in an air atmosphere to obtain the nickel-zinc ferrite magnetic core (the size and specification are the same as those of the embodiment 1).
And (3) performance testing:
the nickel-zinc-ferrite cores of examples 1 to 3 and comparative examples 1 to 3 were subjected to performance tests, the results of which are shown in the following table:
TABLE 1 Performance test results of the nickel-zinc-ferrite cores of examples 1 to 3 and comparative examples 1 to 3
Figure BDA0003653057020000061
Figure BDA0003653057020000071
Note:
inductance value: testing by adopting a precise electromagnetic analyzer 3260B, wherein the testing frequency is 1MHz;
strength of magnetic core: an electronic universal tester is used for testing the strength of the blade by adopting a blade strength testing pressure head (square 0.5mm multiplied by 0.4 mm), the pressing speed is less than or equal to 10mm/min, and the blade strength is tested by pressurizing along the vertical direction of the blade.
As can be seen from Table 1: the nickel-zinc-ferrite cores of examples 1 to 3 have both a high inductance value and a high strength, while the nickel-zinc-ferrite cores of comparative examples 1 to 3, which use the same magnetic powder as the nickel-zinc-ferrite cores of examples 1 to 3, cannot achieve both a high inductance value and a high strength.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A preparation method of a nickel-zinc ferrite magnetic core is characterized by comprising the following steps:
1) Mixing Fe 2 O 3 Mixing the powder, znO powder and NiO powder to obtain magnetic powder;
2) Mixing magnetic powder, polyvinyl alcohol and silica sol, and pressing to obtain a prefabricated blank;
3) Pre-burning the prefabricated blank body and then crushing to obtain pre-burned magnetic powder;
4) Pre-burning magnetic powder and SiO 2 -B 2 O 3 -Al 2 O 3 Mixing the glass powder and then performing ball milling to obtain blended powder;
5) Mixing the blended powder, carbonate, polyvinyl alcohol and a coupling agent, and then granulating to obtain granules;
6) Injecting the granules into a mold to be pressed into a magnetic core blank, and sintering to obtain the nickel-zinc ferrite magnetic core;
the magnetic powder in the step 1) comprises the following components in percentage by mass: fe 2 O 3 Powder: 62 to 72 percent; znO powder: 10 to 13 percent; niO powder: 18 to 25 percent;
step 3) the particle size of the pre-sintered magnetic powder is 1-5 mu m;
step 4) SiO 2 -B 2 O 3 -Al 2 O 3 The adding amount of the glass powder is 0.1-1.0% of the mass of the pre-sintered magnetic powder;
step 4) SiO 2 -B 2 O 3 -Al 2 O 3 The glass powder comprises the following components in percentage by mass: siO 2 2 :50%~65%;B 2 O 3 :10%~15%;Al 2 O 3 :25%~35%;
Step 4) the SiO 2 -B 2 O 3 -Al 2 O 3 The average grain diameter of the glass powder is 0.8-2.0 μm.
2. The method of preparing a nickel zinc ferrite core according to claim 1, wherein: step 2), the addition amount of the polyvinyl alcohol is 1.0-3.0% of the mass of the magnetic powder; and step 2), the mass ratio of the polyvinyl alcohol to the silica sol is 1-4.
3. The method of manufacturing a nickel zinc ferrite core according to claim 1 or 2, characterized in that: and 3) presintering in air atmosphere, wherein the presintering temperature is 950-1100 ℃, and the presintering time is 2-4 h.
4. The method of manufacturing a nickel zinc ferrite core according to claim 1 or 2, characterized in that: step 5), the addition amount of the carbonate is 0.01-0.50% of the mass of the blended powder; step 5), the addition amount of the polyvinyl alcohol is 1.0-3.0% of the total mass of the blending powder and the carbonate; the adding amount of the coupling agent in the step 5) is 0.01-0.10% of the total mass of the blending powder and the carbonate.
5. The method of manufacturing a nickel zinc ferrite core according to claim 1 or 2, characterized in that: and 6) sintering in an air atmosphere, wherein the sintering temperature is 1100-1200 ℃, and the sintering time is 1-3 h.
6. A nickel-zinc-ferrite core, characterized in that it is produced by the production method according to any one of claims 1 to 5.
7. An inductive component, characterized in that the composition comprises a nickel-zinc-ferrite core according to claim 6.
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