CN113307616A - Co2Preparation method of Z-type ferrite sintered sheet - Google Patents

Co2Preparation method of Z-type ferrite sintered sheet Download PDF

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CN113307616A
CN113307616A CN202110527759.5A CN202110527759A CN113307616A CN 113307616 A CN113307616 A CN 113307616A CN 202110527759 A CN202110527759 A CN 202110527759A CN 113307616 A CN113307616 A CN 113307616A
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sintering
type ferrite
ferrite sintered
sintered sheet
preparation
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史慧刚
吴科
蔡庚轩
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Lanzhou University
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Lanzhou University
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Abstract

The invention discloses a Co2The preparation method of the Z-type ferrite sintered sheet comprises the following steps: 1) according to BaxSr3‑ xCo2FeyO41Mixing a barium source, a strontium source, a cobalt source and an iron source, performing first ball milling, performing first sintering, and performing second ball milling to obtain powder; wherein x is more than or equal to 1 and less than or equal to 2; y is more than or equal to 21.6 and less than or equal to 24; 2) mixing the powder obtained in the step 1) with a binder, carrying out third ball milling, and carrying out tape casting on the obtained material to obtain a green body; 3) and 2) sintering the green body obtained in the step 2) for the second time. The present invention provides Co2The preparation method of the Z-type ferrite sintered sheet has simple process,The method has the advantages of convenient operation, good magnetic property of the prepared ferrite sintered sheet, capability of meeting the application requirement under high frequency and wide market prospect.

Description

Co2Preparation method of Z-type ferrite sintered sheet
Technical Field
The invention relates to the technical field of magnetic materials, in particular to Co2A preparation method of Z-type ferrite sintered sheets.
Background
With the development of information technology, electronic devices and devices are developed toward miniaturization, light weight and integration, and the working frequency of passive devices (such as inductors) in the electronic devices is also continuously developed toward high frequency, so that the soft magnetic ferrite material capable of being applied to higher frequency is urgently needed. In terms of classification, the spinel type soft magnetic ferrite and the planar hexagonal crystal type soft magnetic ferrite are mainly widely applied at present. Among them, spinel type soft magnetic ferrites, such as: Mn-Zn and Ni-Zn ferrites are limited by the Snoek limit, and therefore the frequency of use is 300MHz or less.
Because the crystal of the Z-type plane hexagonal soft magnetic ferrite has two different magnetocrystalline anisotropy fields, and the anisotropy field from the outside of the superior plane is far larger than the anisotropy field from the inside of the superior plane, the limit of the Snoek limit can be broken through, and the natural resonance frequency of the Z-type plane hexagonal soft magnetic ferrite is nearly one order of magnitude higher than that of the spinel type soft magnetic ferrite. The Z-shaped plane hexagonal ferrite has the advantages of high initial permeability, high Curie temperature, high resonance frequency, high chemical stability at normal temperature, high mechanical strength and the like, and becomes the first choice for researching ultrahigh frequency ferrite materials.
Common preparation methods of ferrite thin films include Physical Vapor Deposition (PVD), Chemical Vapor Deposition (CVD), Molecular Beam Epitaxy (MBE), deposition sputtering, laser pulse deposition (PLD), and the like. However, the ferrite films prepared by these methods are very thin, typically below 1 μm, and are too thin for most devices in high frequency applications.
Disclosure of Invention
The present invention is directed to solving at least one of the above problems in the prior art. Therefore, one of the objectives of the present invention is to provide a Co2A preparation method of a Z-type ferrite sintered sheet; the second purpose of the invention is to provide Co prepared by the preparation method2Sintering the Z-type ferrite into sheets; it is a further object of the present invention to provide such Co2The application of the Z-type ferrite sintered sheet.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a first aspect of the present invention provides a Co2The preparation method of the Z-type ferrite sintered sheet comprises the following stepsThe method comprises the following steps:
1) according to BaxSr3-xCo2FeyO41Mixing a barium source, a strontium source, a cobalt source and an iron source, performing first ball milling, performing first sintering, and performing second ball milling to obtain powder; wherein x is more than or equal to 1 and less than or equal to 2; y is more than or equal to 21.6 and less than or equal to 24;
2) mixing the powder obtained in the step 1) with a binder, carrying out third ball milling, and carrying out tape casting on the obtained material to obtain a green body;
3) sintering the green body obtained in the step 2) for the second time to obtain Co2And sintering the Z-type ferrite into a sheet.
According to some embodiments of the method of preparing of the present invention, in the step 1), BaxSr3-xCo2FeyO41In the formula, x is 1.5 and y is 21.6.
According to some embodiments of the preparation method of the present invention, in the step 1), the barium source, the strontium source, the cobalt source, and the iron source are subjected to a drying pretreatment before use. In some specific embodiments of the present invention, the drying is specifically performed at 110 ℃ to 125 ℃; the drying time is 8 to 12 hours.
According to some embodiments of the method of manufacturing of the present invention, in step 1), the barium source includes at least one of barium carbonate and barium oxide.
According to some embodiments of the invention, in step 1), the barium source is BaCO3。
According to some embodiments of the preparation method of the present invention, in step 1), the strontium source includes at least one of strontium carbonate and strontium oxide.
According to some embodiments of the invention, in step 1), the strontium source is SrCO3。
According to some embodiments of the preparation method of the present invention, in the step 1), the cobalt source includes at least one of cobalt oxide and cobalt carbonate.
According to some embodiments of the invention, in step 1), the cobalt source is Co3O4。
According to some embodiments of the method of manufacturing of the present invention, in the step 1), the iron source includes at least one of iron oxide and iron carbonate.
According to some embodiments of the invention, in step 1), the iron source is Fe2O3。
According to some embodiments of the manufacturing method of the present invention, in the step 1), a sintering final temperature of the first sintering is 1250 ℃ to 1350 ℃.
According to some embodiments of the invention, in the step 1), the sintering final temperature of the first sintering is 1280 ℃ to 1320 ℃.
According to some embodiments of the preparation method of the present invention, in the step 1), the temperature increase rate of the first sintering is 4 ℃/min to 6 ℃/min.
According to some embodiments of the invention, in the step 1), the temperature increase rate of the first sintering is 4.5 ℃/min to 5.5 ℃/min.
According to some embodiments of the method of manufacturing of the present invention, in the step 1), the time for the first sintering is 3 hours to 5 hours.
According to some embodiments of the method of manufacturing of the present invention, in the step 2), the binder includes at least one of a polyurethane binder, a polysiloxane binder, and polyvinyl alcohol.
According to some embodiments of the invention, in step 2), the binder is a polyurethane binder.
According to some embodiments of the preparation method of the present invention, in the step 2), the mass of the binder is 5% to 11% of the mass of the powder.
According to some embodiments of the invention, in step 2), the mass of the binder is 5% to 8% of the mass of the powder.
According to some embodiments of the preparation method of the present invention, the step 2) further comprises defoaming the material obtained by the third ball milling before casting. In some embodiments of the invention, the method of defoaming is vacuum defoaming; the defoaming time is 1 to 3 hours.
According to some embodiments of the method of manufacturing of the present invention, in the step 2), the casting process temperature is 100 ℃ to 120 ℃.
According to some embodiments of the production method of the present invention, in the step 2), the running speed of the cast slab is 0.4m/min to 0.6 m/min.
According to some embodiments of the method of manufacturing of the present invention, in step 2), the green body has a thickness of 80 to 120 micrometers.
According to some embodiments of the invention, the thickness of the green body in step 2) is between 90 and 110 microns.
According to some embodiments of the preparation method of the present invention, the conditions of the first ball milling, the second ball milling and the third ball milling are as follows: the material-ball ratio is 1: (8-12); the mass ratio of the ball milling medium to the ball milling raw material is 1: (0.8 to 1.2); the ball milling medium is water; the ball is a steel ball.
According to some embodiments of the method of manufacturing of the present invention, in the step 3), the sintering final temperature of the second sintering is 1100 ℃ to 1200 ℃.
According to some embodiments of the method of manufacturing of the present invention, in the step 3), the sintering final temperature of the second sintering is maintained for 5 to 15 hours.
According to some embodiments of the preparation method of the present invention, in the step 3), the second sintering is performed by first heating to 230 ℃ to 280 ℃, and maintaining the temperature for 4 hours to 6 hours, and then heating to 1100 ℃ to 1200 ℃, and maintaining the temperature for 5 hours to 15 hours.
According to some embodiments of the preparation method of the present invention, in the step 3), the temperature increase rate of the second sintering is 0.8 ℃/min to 1.2 ℃/min.
The second aspect of the present invention provides Co obtained by the production method according to the first aspect of the present invention2And sintering the Z-type ferrite into a sheet.
According to some embodiments of the invention, the Co is2The real part of the sintered Z-ferrite sheet has an initial permeability of at least 3.8.
According to other embodiments of the invention, the Co2Of the real part of the sintered Z-type ferrite sheetThe initial magnetic permeability is 3.8-11.5.
According to some embodiments of the invention, the Co is2The resonance frequency of the Z-type ferrite sintered sheet is 2.0 GHz-4 GHz.
According to other embodiments of the invention, the Co2The resonance frequency of the Z-type ferrite sintered sheet is 2.0 GHz-2.5 GHz.
A third aspect of the present invention provides Co2Application of Z-type ferrite sintered sheet in the fields of electronics, communication or control system, and Co2The Z-type ferrite sintered sheet is Co according to the second aspect of the invention2A Z-type ferrite sintered sheet, or made by the method of manufacture of the first aspect of the invention.
The invention has the beneficial effects that:
the present invention provides Co2The preparation method of the Z-shaped ferrite sintered sheet has the advantages of simple process and convenient operation, and the prepared ferrite sintered sheet has good magnetic property, can meet the application requirement under high frequency and has wide market prospect.
Drawings
FIG. 1 shows example 1Co2Scanning electron microscope image of the section of the Z-type ferrite sintered sheet;
FIG. 2 shows Co of example 12Scanning electron microscope images of the surface of the Z-type ferrite sintered sheet;
FIG. 3 shows example 2Co2Scanning electron microscope image of the section of the Z-type ferrite sintered sheet;
FIG. 4 shows example 2Co2Scanning electron microscope images of the surface of the Z-type ferrite sintered sheet;
FIG. 5 shows example 3Co2Scanning electron microscope image of the section of the Z-type ferrite sintered sheet;
FIG. 6 shows example 3Co2Scanning electron microscope images of the surface of the Z-type ferrite sintered sheet;
FIG. 7 shows example 4Co2Scanning electron microscope image of the section of the Z-type ferrite sintered sheet;
FIG. 8 shows example 4Co2Scanning electron microscope images of the surface of the Z-type ferrite sintered sheet;
FIG. 9 shows example 5Co2Z-type ferriteScanning electron microscope images of the sections of the sintered sheets;
FIG. 10 shows example 5Co2Scanning electron microscope images of the surface of the Z-type ferrite sintered sheet;
FIG. 11 shows Co of example 12A dynamic permeability diagram of the Z-type ferrite sintered sheet;
FIG. 12 shows Co of example 12Another dynamic permeability diagram of the Z-type ferrite sintered sheet;
FIG. 13 shows Co at different sintering times2A dynamic permeability diagram of the Z-type ferrite sintered sheet;
FIG. 14 shows Co at different sintering temperatures2Dynamic permeability diagram of Z-type ferrite sintered sheet.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or equipment used in the examples are, unless otherwise specified, either conventionally commercially available or may be obtained by methods known in the art. Unless otherwise indicated, the testing or testing methods are conventional in the art.
Example 1
Example Co2The preparation method of the Z-type ferrite sintered sheet comprises the following steps:
preparing powder: the raw material is analytically pure BaCO3、SrCO3、Fe2O3、Co3O4In proportion of Ba1.5Sr1.5Co2Fe21.6O41The raw materials are firstly put into an oven to be dried for 10 hours at the drying temperature of 120 ℃, are proportioned according to the components and then are put into a ball milling tank to be ball milled, wherein the balls are steel balls (the material-ball ratio is 1: 10, the ball milling medium is water, and the mass ratio of the ball milling medium to the raw materials is 1: 1).
And (3) drying the ball-milled powder in an oven at the drying temperature of 120 ℃, putting the dried powder into an alumina crucible, and sintering in a high-temperature furnace at the sintering temperature of 1300 ℃ for 4 hours at the heating rate of 5 ℃/min.
And crushing and grinding the blocks obtained after sintering, and performing secondary ball milling for 5 hours. And drying the powder obtained after ball milling.
Preparation of slurry: adding an adhesive (polyurethane, the mass ratio is 8 wt%), then placing the mixture into a ball milling tank for ball milling for 24 hours, defoaming the ball milled slurry in vacuum for 2 hours, casting by using a casting machine after defoaming, wherein the first-stage heating temperature of the casting is 100 ℃, the second-stage heating temperature is 120 ℃, the blank advancing speed is 0.5m/min, and casting is carried out to obtain a green blank, wherein the thickness of the green blank is about 100 micrometers.
And (3) sintering: utilize laser to cut the unburned bricks that obtains, put into the muffle furnace after the cutting and sinter, specific sintering process is as follows: heating to 250 ℃ and preserving heat for 5 hours, removing glue, heating to 1150 ℃ and preserving heat for 15 hours, wherein the heating rate in the sintering process is 1 ℃/min, and then cooling along with the furnace to obtain Co of the embodiment2And sintering the Z-type ferrite into a sheet.
Example 2
Example Co2The Z-type ferrite sintered sheet was prepared in the same manner as in example 1 except that the second sintering was carried out at a final sintering temperature of 1150 ℃ for 10 hours in this example.
Example 3
Example Co2The Z-type ferrite sintered sheet was prepared in the same manner as in example 1 except that the second sintering was carried out at a final sintering temperature of 1150 ℃ for 5 hours in this example.
Example 4
Example Co2The Z-type ferrite sintered sheet was prepared in the same manner as in example 1 except that the second sintering was carried out at a sintering final temperature of 1100 ℃ for 5 hours in this example, and the rest was the same as in example 1.
Example 5
Example Co2The Z-type ferrite sintered sheet was prepared in the same manner as in example 1 except that the second sintering was carried out at a sintering final temperature of 1200 ℃ for 5 hours in this example.
FIG. 1 and FIG. 2 show Co of example 12Sintering of Z-type ferriteSection and surface scanning electron micrographs of the flakes. FIG. 3 and FIG. 4 show Co of example 22Scanning electron microscope images of the section and the surface of the Z-type ferrite sintered sheet. FIG. 5 and FIG. 6 show examples 3Co2Scanning electron microscope images of the section and the surface of the Z-type ferrite sintered sheet. As can be seen from FIGS. 1-2, the prepared ferrite sintered sheet is compact, has small surface roughness and uniform particle size. The test results in combination with fig. 1-6 show that: as the sintering time increases, the density of the ferrite pieces increases and the grain size gradually increases. The ferrite sheet of example 3 is very porous and small, with an average grain size of between 3-5 μm and no grain growth; the particle size of the embodiment 2 is obviously increased, the average particle size is about 10 mu m, the particle size is more uniform, and the density is improved; the ferrite sheet of example 1 had a high degree of compactness and a uniform particle size with an average particle size of about 15 μm.
The main difference between examples 3 to 5 is the sintering final temperature of the second sintering. FIG. 7 and FIG. 8 show examples 4Co2Scanning electron microscope images of the section and the surface of the Z-type ferrite sintered sheet. FIG. 9 and FIG. 10 show examples 5Co2Scanning electron microscope images of the section and the surface of the Z-type ferrite sintered sheet. As can be seen from the test results of fig. 5-10: the ferrite pieces are relatively uniform in grain size, ranging from 3 to 5 μm, at different sintering temperatures.
FIG. 11 shows Co of example 12A dynamic permeability diagram of a sintered sheet of Z-type ferrite, FIG. 12 shows Co of example 12And another dynamic permeability diagram of the Z-type ferrite sintered sheet. As can be seen from FIGS. 11 to 12, Co obtained in example 12The real part initial value of the magnetic permeability of the Z-type ferrite sintered sheet is about 6, the imaginary part initial value is very small, and the resonance frequency is about 2.1 GHz. According to the results measured by the vector network analyzer, the initial value of fig. 12 fluctuates greatly since the sample is too thin.
FIG. 13 shows Co at different sintering times2The dynamic permeability diagram of the Z-type ferrite sintered sheet corresponds to the test results of example 1 (sintering time 15h), example 2 (sintering time 10h) and example 3 (sintering time 5 h).As can be seen from fig. 13, the sintering time has little effect on the initial permeability of the ferrite sintered sheet. The imaginary part of the permeability of the sample in example 1 is lower at 1GHz, which may be because a large number of pores exist in the ferrite sintered sheet when the sintering time is shorter, resulting in an increase in loss, and as the sintering time increases, the density of the ferrite sintered sheet gradually increases, the porosity is greatly reduced, the size of the particles is more uniform, and the loss at high frequency is reduced, so that the imaginary part of the permeability of the ferrite sintered sheet with larger particles is lower at 1GHz on the contrary.
FIG. 14 shows Co at different sintering temperatures2The dynamic permeability diagrams of the Z-type ferrite sintered sheets correspond to the test results of example 4 (sintering temperature 1100 ℃), example 3 (sintering temperature 1150 ℃) and example 5 (sintering temperature 1200 ℃). As can be seen from fig. 14, the initial permeability of the ferrite sheet after sintering gradually increases as the sintering temperature increases. The real part of the permeability of the samples at all sintering temperatures showed a tendency to increase before 1 GHz. The initial permeability of example 4 was 3.8, and the initial permeability gradually increased to 5.6 (example 3) and 11.5 (example 5) as the sintering temperature was increased. For the imaginary part of permeability, the imaginary part of permeability is lower for all sintered samples at lower frequencies, and as the frequency increases, the imaginary part of permeability begins to rise, with the higher the sintering temperature, the faster the imaginary part of permeability rises. The sample of example 3 performed well, with a high initial permeability, and the imaginary part of the permeability started to rise around 700 MHz.
As can be seen from the above experimental results, the Co provided by the invention2The Z-type ferrite sintered sheet has good magnetic property and wide application prospect in the fields of electronics, communication or control systems and the like.
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 (10)

1. Co2The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: the method comprises the following steps:
1) according to BaxSr3-xCo2FeyO41Mixing a barium source, a strontium source, a cobalt source and an iron source, performing first ball milling, performing first sintering, and performing second ball milling to obtain powder; wherein x is more than or equal to 1 and less than or equal to 2; y is more than or equal to 21.6 and less than or equal to 24;
2) mixing the powder obtained in the step 1) with a binder, carrying out third ball milling, and carrying out tape casting on the obtained material to obtain a green body;
3) sintering the green body obtained in the step 2) for the second time to obtain Co2And sintering the Z-type ferrite into a sheet.
2. Co according to claim 12The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: in the step 1), the sintering final temperature of the first sintering is 1250-1350 ℃.
3. Co according to claim 12The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: in the step 2), the binder comprises at least one of a polyurethane binder, a polysiloxane binder and polyvinyl alcohol.
4. Co according to claim 32The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: in the step 2), the mass of the binder is 5-11% of the mass of the powder.
5. Co according to claim 12The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: in the step 2), the thickness of the green body is 80-120 microns.
6. Co according to claim 12The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: in the step 3), the sintering final temperature of the second sintering is1100℃～1200℃。
7. Co according to claim 62The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: and in the step 3), preserving the heat for 5-15 hours at the final sintering temperature of the second sintering.
8. Co according to claim 62The preparation method of the Z-type ferrite sintered sheet is characterized by comprising the following steps: in the step 3), the temperature rise rate of the second sintering is 0.8 ℃/min to 1.2 ℃/min.
9. Co produced by the production method according to any one of claims 1 to 82And sintering the Z-type ferrite into a sheet.
10.Co2The application of the Z-type ferrite sintered sheet in the fields of electronics, communication or control systems is characterized in that: the Co2The Z-type ferrite sintered sheet is Co as claimed in claim 92A Z-type ferrite sintered sheet or produced by the production method according to any one of claims 1 to 8.
CN202110527759.5A 2021-05-14 2021-05-14 Co2Preparation method of Z-type ferrite sintered sheet Pending CN113307616A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107266062A (en) * 2017-08-03 2017-10-20 中南大学 A kind of anisotropy Co2Z-type hexad ferrite magnetic core and preparation method thereof
CN112624750A (en) * 2021-01-06 2021-04-09 横店集团东磁股份有限公司 Preparation method of Z-shaped hexaferrite material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107266062A (en) * 2017-08-03 2017-10-20 中南大学 A kind of anisotropy Co2Z-type hexad ferrite magnetic core and preparation method thereof
CN112624750A (en) * 2021-01-06 2021-04-09 横店集团东磁股份有限公司 Preparation method of Z-shaped hexaferrite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
OSAMU KIMURA 等: "Enhanced Dispersion Frequency of Hot-Pressed Z-Type Magnetoplumbite Ferrite with the Composition 2CoO•3Ba0.5Sr0.5O•10.8Fe2O3", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 *

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