CN113860864A - High-remanence-ratio high-anisotropy-field SrM microwave ferrite material and preparation method thereof - Google Patents

High-remanence-ratio high-anisotropy-field SrM microwave ferrite material and preparation method thereof Download PDF

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CN113860864A
CN113860864A CN202111180299.XA CN202111180299A CN113860864A CN 113860864 A CN113860864 A CN 113860864A CN 202111180299 A CN202111180299 A CN 202111180299A CN 113860864 A CN113860864 A CN 113860864A
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兰中文
戴越
余忠
孙科
邬传健
蒋晓娜
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University of Electronic Science and Technology of China
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Abstract

A high remanence ratio and high anisotropy field SrM microwave ferrite material and a preparation method thereof belong to the technical field of ferrite material preparation. Comprises a main formula and a dopant, wherein the main formula is made of Fe2O3、SrCO3、La2O3、CaCO3、Co2O3And Al2O3As raw material, according to the chemical formula Sr0.4La0.3Ca0.3Fe11.85‑xAlxCo0.15O19Proportioning, wherein x is 0.3-1.3; the dopant accounts for the weight percentage of the main formula: 0.60 to 1.00 wt% of CaCO3、0.30～0.70wt％SiO2、0.10～0.40wt％H3BO3. The high-remanence-ratio high-anisotropy-ratio SrM microwave ferrite material provided by the invention has the remanence ratio of more than 80%, the anisotropy field of more than 21kOe and the maximum value of 29kOe, and the working frequency of more than 60 GHz.

Description

High-remanence-ratio high-anisotropy-field SrM microwave ferrite material and preparation method thereof
Technical Field
The invention belongs to the technical field of ferrite material preparation, and particularly relates to an anisotropic field SrM microwave ferrite material with high remanence ratio and a preparation method thereof.
Background
In recent years, with the development of electronic information systems toward higher frequencies and smaller sizes, electronic devices such as microwave/millimeter wave isolators, circulators, and the like have been attracting attention in the direction of higher frequencies, smaller sizes, and flatter sizes. For electronic devices, increasing their operating frequency f directly increases the transmission efficiency of data and other advantages, which is why the operating frequency of 5G communication devices is increased to the millimeter wave band. Conventional microwave ferrite devices are typically fabricated using yttrium iron garnet ferrite (YIG ferrite). Since YIG ferrite is a soft magnetic ferrite, its saturation magnetization is 4 π MsAnd an anisotropy field HaThe frequency is low, and the working frequency is 10-18 GHz in practical application.
According to the formula of kittel:
Figure BDA0003296841580000011
wherein f is the working frequency, H is the external constant magnetic field, and Nx，NyAnd NzThe demagnetization factors of the sample in the three directions of the x axis, the y axis and the z axis are respectively, and gamma is the gyromagnetic ratio. If the operating frequency f is continuously increased to the millimeter wave frequency band, the external constant magnetic field H must be increased, which inevitably increases the volume and weight of the microwave device. This is contrary to the development direction of miniaturization, planarization and weight reduction of devices. Therefore, if the remanence ratio and the anisotropy field of the ferrite material are improved, only a small external constant magnetic field H can be added or even the external constant magnetic field H can be removed in the application design of the microwave ferrite device, thereby realizing the device "Self-bias ", thus can reduce the volume and weight of the device, can make the device work in the higher frequency band, meet the high frequency of the device at the same time, miniaturization and level.
Aiming at the research of high remanence ratio and high anisotropy field SrM microwave ferrite, Chengdu information engineering university publishes two SrM microwave ferrite materials: the La-Co substituted SrM microwave ferrite material prepared by microwave sintering has a magnetocrystalline anisotropy field of 19.3kOe and a specific saturation magnetization of 64.6 emu/g; another is Bi2O3·B2O3·SiO2ZnO (BBSZ) additive doped SrM microwave ferrite material has a magnetocrystalline anisotropy field of 19.2kOe and a saturation magnetization of 65.3 emu/g. American Tufts university discloses a SrM microwave ferrite powder material with the powder particle size of 40nm, and the performance indexes of the SrM microwave ferrite powder material are as follows: the magnetocrystalline anisotropy field reaches 17.2kOe, and the working frequency reaches 48.2 GHz.
Based on the above, the current SrM microwave ferrite material is difficult to meet the requirements of microwave magnetic devices for high frequency, miniaturization and light weight development, so the invention provides an anisotropic field SrM microwave ferrite material with high remanence ratio and a preparation method thereof.
Disclosure of Invention
The invention aims to provide an anisotropic field SrM microwave ferrite material with high remanence ratio and a preparation method thereof, aiming at the technical problem that the development requirements of miniaturization, light weight and high frequency of a microwave ferrite device are contradictory to the material performance.
The core idea of the invention is as follows: in the SrM microwave ferrite material, Ca is adopted2+Partially substituted Sr2+To reduce the preparation cost of the material and adopts La3+And Co3+Each being partially substituted for Sr2+And Fe3+To improve the anisotropy of the material, the formula of the whole material system is determined to be Sr0.4La0.3Ca0.3Fe11.85Co0.15O19On this formulation system, Al is used3+Ion pair Fe3+The ions carry out the substitution. Al (Al)3+Four sides of M-type hexagonal strontium ferrite are preferentially replaced by ionsThe crystal position of the body and the octahedron makes the ferrite saturated magnetization 4 pi MsFast reduction and uniaxial anisotropy constant K1The anisotropy field is greatly improved by properly reducing the anisotropy field. According to the formula of kittel:
Figure BDA0003296841580000021
anisotropy field HaThe working frequency f of the material can be improved under the condition of reducing or even removing the external magnetic field H, and the requirements of high frequency, miniaturization and planarization of the device are met.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-remanence-ratio high-anisotropy-field SrM microwave ferrite material comprises a main formula and a dopant, wherein the main formula is Fe2O3、SrCO3、La2O3、CaCO3、Co2O3And Al2O3As raw material, according to the chemical formula Sr0.4La0.3Ca0.3Fe11.85- xAlxCo0.15O19Proportioning, wherein x is 0.3-1.3;
the dopant accounts for the weight percentage of the main formula: 0.60 to 1.00 wt% of CaCO3、0.30～0.70wt％SiO2、0.10～0.40wt％H3BO3。
A preparation method of a high remanence ratio and high anisotropy field SrM microwave ferrite material comprises the following steps:
step 1, formula:
with Fe2O3、SrCO3、La2O3、CaCO3、Co2O3And Al2O3As a raw material, according to the chemical formula Sr0.4La0.3Ca0.3Fe11.85-xAlxCo0.15O19Weighing and mixing the materials according to the proportion; wherein x is 0.3-1.3;
step 2, primary ball milling:
performing primary ball milling on the powder obtained in the step 1, wherein the ball milling time is 3-6 hours;
step 3, pre-burning:
drying the primary ball-milled material obtained in the step 2, and then pre-sintering at the temperature of 1200-1350 ℃ for 1-3 h to obtain Sr0.4La0.3Ca0.3Fe11.85-xAlxCo0.15O19Powder, i.e. the main formulation;
step 4, doping:
adding a doping agent into the powder obtained in the step 3, wherein the doping agent accounts for the main formula by weight percent: 0.60 to 1.00 wt% of CaCO3、0.30～0.70wt％SiO2、0.10～0.40wt％H3BO3；
Step 5, secondary ball milling:
performing secondary ball milling on the powder obtained in the step (4), wherein the ball milling time is 5-7 hours, and the particle size of the powder is controlled to be 1.0-1.3 mu m;
step 6, forming:
pressing and molding the powder obtained in the step 5 under a magnetic field molding machine, wherein the molding pressure is 5-8 MPa, and the molding magnetic field is 6000-10000 Oe;
and 7, sintering:
and (3) sintering the blank obtained after the forming in the step (6) in a sintering furnace at the sintering temperature of 1200-1300 ℃ for 1-4 hours, naturally cooling to room temperature after the sintering is finished, and taking out to obtain the microwave ferrite material.
And (3) performing magnetic property test on the sample prepared in the step (7): the magnetic properties of the material were tested with a vibrating sample magnetometer, model Lake Shore 8604. Tests prove that the high-remanence-ratio high-anisotropy-ratio SrM microwave ferrite material prepared by the invention has the remanence ratio of more than 80 percent, the anisotropy field of more than 21kOe, the maximum value of 29kOe and the working frequency of more than 60 GHz.
Compared with the prior art, the invention has the beneficial effects that:
1. the high-remanence-ratio high-anisotropy-field SrM microwave ferrite material provided by the invention greatly improves the anisotropy field of the material, effectively improves the working frequency of the material under the condition of reducing the external field or even eliminating the external field, and promotes the development of high frequency, miniaturization and light weight of a magnetic microwave device.
2. The high-remanence-ratio high-anisotropy-ratio SrM microwave ferrite material provided by the invention has the remanence ratio of more than 80%, the anisotropy field of more than 21kOe and the maximum value of 29kOe, and the working frequency of more than 60 GHz.
Drawings
FIG. 1 is a scanning electron micrograph of samples obtained in comparative example (a), example 1(b), example 2(c) and example 3 (d).
Detailed Description
The invention is further described with reference to the following figures and detailed description.
The invention provides an SrM microwave ferrite material with a high remanence ratio and an anisotropic field and a preparation method thereof, aiming at the technical problem that the development requirements of miniaturization, light weight and high frequency of a microwave ferrite device are contradictory to the material performance. The guiding idea is as follows: in the SrM microwave ferrite material, Ca is adopted2+Partially substituted Sr2+To reduce the preparation cost of the material and adopts La3 +And Co3+Each being partially substituted for Sr2+And Fe3+To improve the anisotropy of the material, the formula of the whole material system is determined to be Sr0.4La0.3Ca0.3Fe11.85Co0.15O19On this formulation system, Al is utilized3+The ion doping improves the anisotropic field of SrM microwave ferrite, thereby improving the working frequency of the material under the condition of low external field or zero external field and achieving the effect of self-bias.
Examples
A preparation method of a high remanence ratio and high anisotropy field SrM microwave ferrite material comprises the following steps:
step 1, formula:
with Fe2O3、SrCO3、La2O3、CaCO3、Co2O3And Al2O3As a raw material, is prepared byAccording to the chemical formula Sr0.4La0.3Ca0.3Fe11.85-xAlxCo0.15O19Weighing and mixing the materials according to the proportion;
examples Comparative example Example 1 Example 2 Example 3
x 0.0 0.4 0.8 1.2
Fe2O3 173.77g 169.69g 165.52g 161.26g
SrCO3 10.88g 11.00g 11.12g 11.24g
La2O3 8.92g 9.02g 9.11g 9.21g
Co2O3 2.29g 2.32g 2.34g 2.37g
CaCO3 5.51g 5.57g 5.63g 5.69g
Al2O3 0.00g 3.38g 7.84g 11.89g
Step 2, primary ball milling:
performing primary ball milling on the powder obtained in the step 1 for 4 hours;
step 3, pre-burning:
drying the primary ball-milled material obtained in the step 2, and then pre-sintering at 1300 ℃ for 2h to obtain Sr0.4La0.3Ca0.3Fe11.85-xAlxCo0.15O19Powder, i.e. the main formulation;
step 4, doping:
adding an additive into the powder obtained in the step 3, wherein the additive accounts for the following main formula in percentage by weight: 0.80 wt% CaCO3、0.50wt％SiO2、0.20wt％H3BO3；
Step 5, secondary ball milling:
performing secondary ball milling on the powder obtained in the step (4), wherein the ball milling time is 6 hours, and the particle size of the powder is controlled to be 1.0-1.3 mu m;
step 6, forming:
pressing and molding the powder obtained in the step 5 under a magnetic field molding machine, wherein the molding pressure is 6MPa, and the molding magnetic field is 8000 Oe;
and 7, sintering:
and (3) sintering the blank obtained after the forming in the step (6) in a sintering furnace at the sintering temperature of 1220 ℃ for 2 hours, naturally cooling to room temperature after the sintering is finished, and taking out the blank to obtain the microwave ferrite material.
The SrM microwave ferrite material prepared by the process has the following performance indexes:
the test results of the comparative example and the examples 1 to 3 are as follows:
Figure BDA0003296841580000051
FIG. 1 is a scanning electron micrograph of samples obtained in comparative example (a), example 1(b), example 2(c) and example 3 (d). As can be seen from FIG. 1, the average grain size of the sample decreased and the density decreased as the amount of Al ion substitution increased. Since the substitution of the Al ions for the Fe ions increases the activation energy required for sintering the sample, the increase in the substitution amount of the Al ions leads to a decrease in the rate of grain growth, resulting in a decrease in the average grain size.

Claims (2)

1. A high-remanence-ratio high-anisotropy-field SrM microwave ferrite material comprises a main formula and a dopant, wherein the main formula is Sr0.4La0.3Ca0.3Fe11.85-xAlxCo0.15O19，x＝0.3～1.3；
The dopant accounts for the weight percentage of the main formula: 0.60 to 1.00 wt% of CaCO3、0.30～0.70wt％SiO2、0.10～0.40wt％H3BO3。
2. A preparation method of a high remanence ratio and high anisotropy field SrM microwave ferrite material comprises the following steps:
step 1, formula:
with Fe2O3、SrCO3、La2O3、CaCO3、Co2O3And Al2O3As a raw material, according to the chemical formula Sr0.4La0.3Ca0.3Fe11.85- xAlxCo0.15O19Weighing and mixing the materials according to the proportion; wherein x is 0.3-1.3;
step 2, primary ball milling:
performing primary ball milling on the powder obtained in the step 1, wherein the ball milling time is 3-6 hours;
step 3, pre-burning:
drying the primary ball-milled material obtained in the step 2, and then pre-sintering at 1200-1350 ℃ for 1-3 h to obtain a main material;
step 4, doping:
adding a doping agent into the powder obtained in the step 3, wherein the doping agent accounts for the main materials in percentage by weight: 0.60 to 1.00 wt% of CaCO3、0.30～0.70wt％SiO2、0.10～0.40wt％H3BO3；
Step 5, secondary ball milling:
performing secondary ball milling on the powder obtained in the step (4), wherein the ball milling time is 5-7 hours, and the particle size of the powder is controlled to be 1.0-1.3 mu m;
step 6, forming:
pressing and forming the powder obtained in the step (5), wherein the forming pressure is 5-8 MPa, and the forming magnetic field is 6000-10000 Oe;
and 7, sintering:
and (3) sintering the blank obtained after the forming in the step (6), wherein the sintering temperature is 1200-1300 ℃, the sintering time is 1-4 hours, after the sintering is finished, naturally cooling to room temperature, and taking out to obtain the microwave ferrite material.
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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN114409392A (en) * 2022-01-21 2022-04-29 电子科技大学 High-remanence-ratio low-loss composite hexagonal ferrite material and preparation method thereof
CN115385679A (en) * 2022-08-30 2022-11-25 西南应用磁学研究所(中国电子科技集团公司第九研究所) Strontium ferrite material with high remanence ratio, high coercivity and low ferromagnetic resonance line width and preparation method thereof
CN115477534A (en) * 2022-10-20 2022-12-16 电子科技大学 Double-phase composite ferrite material for Ku waveband self-bias device and preparation method thereof
CN116969751A (en) * 2023-08-24 2023-10-31 电子科技大学 High-resistance high-magnetic-property hexagonal ferrite material and preparation method thereof
CN116969751B (en) * 2023-08-24 2024-10-29 电子科技大学 High-resistance high-magnetic-property hexagonal ferrite material and preparation method thereof

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US5648039A (en) * 1992-04-24 1997-07-15 Tdk Corporation Process for the production of anisotropic ferrite magnets
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CN115477534A (en) * 2022-10-20 2022-12-16 电子科技大学 Double-phase composite ferrite material for Ku waveband self-bias device and preparation method thereof
CN115477534B (en) * 2022-10-20 2023-03-28 电子科技大学 Double-phase composite ferrite material for Ku waveband self-bias device and preparation method thereof
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