1. A ferrite material suitable for miniaturized microwave devices is characterized in that the ferrite material has a chemical formula of Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Wherein a is more than or equal to 0.5 and less than or equal to 1, b is more than or equal to 0.1 and less than or equal to 0.3, c is more than or equal to 0.1 and less than or equal to 0.4, d is more than or equal to 0.2 and less than or equal to 0.4, and e is more than or equal to 0.1 and less than or equal to 0.2.

2. The ferrite material of claim 1, wherein the sum of a and b is 0.6-1.2.

3. The ferrite material of claim 1 or 2, wherein the sum of c, d and e is 0.4-0.8.

4. A method of preparing a ferrite material as claimed in any of claims 1 to 3, characterized in that said method comprises the steps of:

(1) performing primary ball milling on the mixed raw materials according to the formula amount to obtain a mixture;

(2) calcining the mixture obtained in the step (1) in an oxygen atmosphere to obtain a pre-calcined material;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder;

(5) and (4) performing compression molding on the ferrite powder obtained in the step (4), and sintering to obtain the ferrite material.

5. The method according to claim 4, wherein the raw material of the step (1) comprises Y₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃；

Preferably, the dispersing agent used in the primary ball milling in the step (1) comprises water and/or absolute ethyl alcohol;

preferably, the ball milling medium used in the primary ball milling in the step (1) comprises zirconium balls and/or steel balls;

preferably, the average grain diameter of the mixture obtained in the step (1) is 3-5 μm.

6. The production method according to claim 4 or 5, wherein the oxygen atmosphere of the step (2) has an oxygen concentration of 80 to 100 vol%;

preferably, the absolute pressure of the oxygen atmosphere in the step (2) is 0.1-0.5 MPa;

preferably, the temperature of the calcination in the step (2) is 900-1100 ℃;

preferably, the calcination time of the step (2) is 4-6 h.

7. The preparation method according to any one of claims 4 to 6, wherein the dispersant used in the secondary ball milling in step (3) comprises water and/or absolute ethyl alcohol;

preferably, the ball milling medium used in the secondary ball milling in the step (3) comprises zirconium balls and/or steel balls;

preferably, the average particle size of the ball grinding material obtained in the step (3) is 5-10 μm.

8. The method according to any one of claims 4 to 7, wherein the binder of step (4) comprises an aqueous solution of polyvinyl alcohol and/or carboxymethyl cellulose;

preferably, the addition amount of the binder in the step (4) is 0.4-0.8 wt% of the ferrite powder;

preferably, the average particle size of the ferrite powder obtained in step (4) is 20 to 40 μm.

9. The production method according to any one of claims 4 to 8, wherein the press molding in the step (5) is cold isostatic pressing, and the applied pressure is 100-200 MPa;

preferably, the sintering temperature in the step (5) is 1300-1500 ℃;

preferably, the sintering time in the step (5) is 4-6 h.

10. The method of any one of claims 4 to 9, comprising the steps of:

(1) performing primary ball milling on the mixed raw materials according to the formula amount to obtain a mixture with the average particle size of 3-5 mu m; the dispersing agent adopted by the primary ball milling comprises water and/or absolute ethyl alcohol, and the ball milling medium comprises zirconium balls and/or steel balls; the raw material comprises Y₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃；

(2) Calcining the mixture obtained in the step (1) for 4-6h at 900-;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material with the average particle size of 5-10 microns; the dispersing agent adopted by the secondary ball milling comprises water and/or absolute ethyl alcohol, and the ball milling medium comprises zirconium balls and/or steel balls;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder with the average particle size of 20-40 mu m; the binder comprises polyvinyl alcohol aqueous solution and/or carboxymethyl cellulose, and the addition amount of the binder is 0.4-0.8 wt% of the ferrite powder;

(5) and (4) applying cold isostatic pressing with the pressure of 100-200MPa to the ferrite powder obtained in the step (4), and sintering at 1300-1500 ℃ for 4-6h to obtain the ferrite material.

Background

Microwave ferrite materials and devices are developed in the fifth and sixty years of the twentieth century, and have been widely applied to aspects of national defense electronics, satellite communication, mobile communication and the like after decades of development. In a long period of time, the microwave engineering field continuously puts forward new requirements for high power characteristics, low loss characteristics and the like of microwave devices, but the requirement for miniaturization of the microwave devices is not urgent, which also leads scientific research technicians to devote long time to improving the high power bearing capacity of ferrite materials and reducing the ferromagnetic resonance line width of the materials, but rarely considers whether the ferrite materials can meet the requirement for miniaturization of the devices.

In recent years, with the rapid development of 5G communication technology, the demand for miniaturization and weight reduction of devices is more and more urgent, and the size and weight reduction of ferrite components is particularly important because the ferrite components are much larger than other components.

Researchers in the field find that the dielectric constant epsilon, which is one of the main parameters of device design, is closely related to the device size. Since the wavelength of a medium through which an electromagnetic wave propagates in the medium is inversely proportional to the square root of the dielectric constant, increasing the dielectric constant of a material is an important means for realizing miniaturization of a microwave device.

CN 107021747A discloses a high-temperature co-firing method of microwave ferrite material and microwave dielectric ceramic, which regulates and controls the sintering temperature, densification rate, sintering shrinkage and thermal expansion rate of two ceramic materials by adding auxiliary agent, adjusting the particle size of raw material, inserting transition layer and controlling the thickness of green film, and reduces the defects of warpage, spalling, crack and the like generated by high-temperature co-firing; secondly, obtaining a high-quality raw porcelain band by optimizing a tape casting process; and finally, high-temperature co-firing is carried out by a space limitation sintering method, so that internal stress is uniformly released, and the generation of micro defects at a ceramic composite interface is reduced or inhibited. Although the method solves the problem of serious mismatching of the co-firing of the microwave dielectric ceramic material and the microwave ferrite material, the high-temperature matching co-firing of 3-30 layers of microwave dielectric ceramic and the microwave ferrite material is realized, and a material foundation is laid for further miniaturization of a multi-layer high-temperature and low-temperature co-firing microwave device; however, the dielectric constant of the prepared ferrite material is not large enough, and the problem that the size cannot be reduced to meet the requirement of a 5G base station isolator is caused.

CN 111285673A discloses a high dielectric constant microwave ferrite material, a preparation method and a microwave communication device, wherein the chemical formula of the microwave ferrite material is Bi_1.25Ca_0.25+2xY_1.5-2xZr_0.25Al_xMn_yFe_4.75-x-yX is more than or equal to 0.05 and less than or equal to 0.3, y is more than or equal to 0.05 and less than or equal to 0.15, the preparation method of the high dielectric constant microwave ferrite material prepares the raw materials according to the stoichiometric ratio of the molecular formula, and the raw materials are subjected to wet ball-milling mixing, drying and sieving, pre-sintering, wet ball-milling and grinding, spray granulation, press molding and sintering in sequence to obtain the microwave ferrite material with the dielectric constant of about 28, the 4 pi Ms is 1850-_cMicrowave ferrite material at 200 deg.C or higher. Although the dielectric constant of the microwave ferrite material is high, the ferromagnetic resonance line width of the microwave ferrite material is also large, the ferromagnetic resonance line width is an important factor influencing microwave transmission loss, and the larger the ferromagnetic resonance line width is, the more microwave signals are lost in the transmission process in a microwave device, so that the ferrite loses practical value in a miniaturized microwave device.

Therefore, how to provide a ferrite material suitable for a miniaturized microwave device and a preparation method thereof can improve the dielectric constant of the ferrite, ensure that the ferromagnetic resonance line width is not too large, and reduce the electromagnetic loss, thereby clearing obstacles for miniaturization and light weight of communication devices and becoming a problem which needs to be solved by technical personnel in the field at present.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a ferrite material suitable for a miniaturized microwave device and a preparation method thereof.

In order to achieve the purpose, the invention adopts the following technical scheme:

in a first aspect, the present invention provides a ferrite material suitable for miniaturized microwave devices, a set of said ferrite materialsHas the chemical formula of Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Wherein a is more than or equal to 0.5 and less than or equal to 1, b is more than or equal to 0.1 and less than or equal to 0.3, c is more than or equal to 0.1 and less than or equal to 0.4, d is more than or equal to 0.2 and less than or equal to 0.4, and e is more than or equal to 0.1 and less than or equal to 0.2.

The ferrite material provided by the invention is garnet type ferrite material Y₃Fe₅O₁₂Prepared on the basis of Ti by means of ion exchange⁴⁺、Zr⁴⁺、Sn⁴⁺With Ge⁴⁺In synergy, by partial substitution of Fe³⁺The ferromagnetic resonance line width of the obtained ferrite material is reduced, and the problem of overlarge ferromagnetic resonance line width caused by the addition of Bi is avoided; ca²⁺By partial substitution of Y³⁺The dielectric constant of the obtained ferrite material is improved, so that the obtained ferrite material has higher saturation magnetization, and the electromagnetic loss of the ferrite material applied to a miniaturized microwave device is reduced.

In the invention, the miniaturized microwave device is a microwave device with the circulator diameter being less than 7 mm.

In the present invention, a is 0.5 to 1, and may be, for example, 0.5, 0.55, 0.6, 0.65, 0.7, 0.75, 0.8, 0.85, 0.9, 0.95 or 1, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned numerical range are also applicable.

In the present invention, b is 0.1 to 0.3, and may be, for example, 0.1, 0.12, 0.14, 0.16, 0.18, 0.2, 0.22, 0.24, 0.26, 0.28 or 0.3, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are also applicable.

In the present invention, c is 0.1 to 0.4, and may be, for example, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35 or 0.4, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.

In the present invention, d is 0.2 to 0.4, and may be, for example, 0.2, 0.22, 0.24, 0.26, 0.28, 0.3, 0.32, 0.34, 0.36, 0.38 or 0.4, but is not limited to the above-mentioned values, and other values not mentioned in the numerical range are also applicable.

In the present invention, e is 0.1 to 0.2, and may be, for example, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19 or 0.2, but is not limited to the above-mentioned values, and other values not mentioned in the numerical range are also applicable.

Preferably, the sum of a and b is 0.6 to 1.2, and may be, for example, 0.6, 0.65, 0.7, 0.75, 0.8, 0.85, 0.9, 0.95, 1, 1.1 or 1.2, but is not limited to the recited values, and other unrecited values within the range of values are equally applicable.

Preferably, the sum of c, d and e is 0.4 to 0.8, and may be, for example, 0.4, 0.45, 0.5, 0.55, 0.6, 0.65, 0.7, 0.75 or 0.8, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.

In a second aspect, the present invention provides a method for preparing the ferrite material according to the first aspect, the method comprising the steps of:

(1) performing primary ball milling on the mixed raw materials according to the formula amount to obtain a mixture;

(2) calcining the mixture obtained in the step (1) in an oxygen atmosphere to obtain a pre-calcined material;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder;

(5) and (4) performing compression molding on the ferrite powder obtained in the step (4), and sintering to obtain the ferrite material.

The preparation method provided by the invention prepares the pre-sintering material by carrying out oxygenation and calcination on the mixture, and prepares Fe²⁺Is oxidized into Fe^{3 +}Inhibit Fe²⁺Thereby weakening the super exchange effect strength in the obtained ferrite material, reducing the ferromagnetic resonance line width, improving the resistivity and reducing the dielectric loss.

Preferably, the raw material of step (1) comprises Y₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃。

Preferably, the dispersant used in the primary ball milling in step (1) comprises water and/or absolute ethyl alcohol.

Preferably, the ball milling medium used in the primary ball milling in the step (1) comprises zirconium balls and/or steel balls.

Preferably, the mixture obtained in step (1) has an average particle size of 3 to 5 μm, and may be, for example, 3 μm, 3.2 μm, 3.4 μm, 3.6 μm, 3.8 μm, 4 μm, 4.2 μm, 4.4 μm, 4.6 μm, 4.8 μm or 5 μm, but is not limited to the values listed, and other values not listed in this range are also applicable.

Preferably, the oxygen concentration of the oxygen atmosphere in step (2) is 80 to 100 vol%, for example, 80 vol%, 82 vol%, 84 vol%, 86 vol%, 88 vol%, 90 vol%, 92 vol%, 94 vol%, 96 vol%, 98 vol% or 100 vol%, but not limited to the recited values, and other values not recited in the numerical range are also applicable.

Preferably, the absolute pressure of the oxygen atmosphere in step (2) is 0.1 to 0.5MPa, and may be, for example, 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, 0.3MPa, 0.35MPa, 0.4MPa, 0.45MPa or 0.5MPa, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.

Preferably, the temperature of the calcination in step (2) is 900-.

Preferably, the calcination in step (2) is carried out for 4-6h, for example, 4h, 4.2h, 4.4h, 4.6h, 4.8h, 5h, 5.2h, 5.4h, 5.6h, 5.8h or 6h, but not limited to the recited values, and other values not recited in the range of values are also applicable.

Preferably, the dispersant used in the secondary ball milling in step (3) comprises water and/or absolute ethyl alcohol.

Preferably, the ball milling medium used in the secondary ball milling in the step (3) comprises zirconium balls and/or steel balls.

Preferably, the average particle size of the ball mill obtained in step (3) is 5 to 10 μm, and may be, for example, 5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm, 8 μm, 8.5 μm, 9 μm, 9.5 μm or 10 μm, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.

Preferably, the binder of step (4) comprises an aqueous solution of polyvinyl alcohol and/or carboxymethyl cellulose.

Preferably, the binder of step (4) is added in an amount of 0.4-0.8 wt% of the ferrite powder, for example, 0.4 wt%, 0.45 wt%, 0.5 wt%, 0.55 wt%, 0.6 wt%, 0.65 wt%, 0.7 wt%, 0.75 wt%, or 0.8 wt%, but is not limited to the recited values, and other values not recited in the range of the recited values are also applicable.

Preferably, the ferrite powder obtained in step (4) has an average particle size of 20 to 40 μm, for example, 20 μm, 22 μm, 24 μm, 26 μm, 28 μm, 30 μm, 32 μm, 34 μm, 36 μm, 38 μm or 40 μm, but is not limited to the values listed, and other values not listed in this range are also applicable.

Preferably, the press forming in step (5) is a cold isostatic press with an applied pressure of 100 and 200MPa, such as 100MPa, 110MPa, 120MPa, 130MPa, 140MPa, 150MPa, 160MPa, 170MPa, 180MPa, 190MPa or 200MPa, but not limited to the recited values, and other unrecited values within the range are equally applicable.

Preferably, the sintering temperature in step (5) is 1300-1500 ℃, and may be, for example, 1300 ℃, 1320 ℃, 1340 ℃, 1360 ℃, 1380 ℃, 1400 ℃, 1420 ℃, 1440 ℃, 1460 ℃, 1480 ℃ or 1500 ℃, but is not limited to the recited values, and other values not recited within the range are equally applicable.

Preferably, the sintering time in step (5) is 4-6h, for example, 4h, 4.2h, 4.4h, 4.6h, 4.8h, 5h, 5.2h, 5.4h, 5.6h, 5.8h or 6h, but is not limited to the recited values, and other values not recited in the range of values are also applicable.

As a preferable technical solution of the second aspect of the present invention, the preparation method comprises the steps of:

(1) performing primary ball milling on the mixed raw materials according to the formula amount to obtain a mixture with the average particle size of 3-5 mu m; the dispersing agent adopted by the primary ball milling comprises water and/or absolute ethyl alcohol, and the ball milling medium comprises zirconium balls and/or steel balls; the raw material comprises Y₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃；

(2) Calcining the mixture obtained in the step (1) for 4-6h at 900-;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material with the average particle size of 5-10 microns; the dispersing agent adopted by the secondary ball milling comprises water and/or absolute ethyl alcohol, and the ball milling medium comprises zirconium balls and/or steel balls;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder with the average particle size of 20-40 mu m; the binder comprises polyvinyl alcohol aqueous solution and/or carboxymethyl cellulose, and the addition amount of the binder is 0.4-0.8 wt% of the ferrite powder;

(5) and (4) applying cold isostatic pressing with the pressure of 100-200MPa to the ferrite powder obtained in the step (4), and sintering at 1300-1500 ℃ for 4-6h to obtain the ferrite material.

Compared with the prior art, the invention has the beneficial effects that:

(1) the invention provides a chemical formula of Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂The ferrite material is garnet type ferrite material Y₃Fe₅O₁₂Prepared on the basis of Ti by means of ion exchange⁴⁺、Zr⁴⁺、Sn⁴⁺With Ge⁴⁺In synergy, by partial substitution of Fe³⁺The ferromagnetic resonance line width of the obtained ferrite material is reduced, and the problem of overlarge ferromagnetic resonance line width caused by the addition of Bi is avoided; ca²⁺By partial substitution of Y³⁺Improve the instituteThe dielectric constant of the ferrite material is obtained, so that the ferrite material has higher saturation magnetization, and the electromagnetic loss of the ferrite material when the ferrite material is applied to a miniaturized microwave device is reduced;

(2) the preparation method provided by the invention prepares the pre-sintering material by carrying out oxygenation and calcination on the mixture, and prepares Fe²⁺Is oxidized into Fe³⁺Inhibit Fe²⁺The generation of the ferrite reduces the super exchange effect strength in the obtained ferrite material, reduces the ferromagnetic resonance line width, improves the resistivity and reduces the dielectric loss;

(3) the dielectric constant of the ferrite material obtained by the invention is not lower than 20, the ferromagnetic resonance line width is not more than 30Oe, the Curie temperature can reach more than 250 ℃, the saturation magnetization can reach more than 1680Gs, and the ferrite material is particularly suitable for miniaturized microwave devices.

Detailed Description

The technical solution of the present invention is further explained by the following embodiments.

Example 1

This example provides a ferrite material suitable for miniaturized microwave devices, and the chemical formula of the ferrite material is Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.9, b is 0.2, c is 0.25, d is 0.3, and e is 0.15. The preparation method comprises the following steps:

(1) carrying out primary ball milling and mixing Y according to the formula amount₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃To obtain a mixture with the average grain diameter of 4 mu m; the dispersing agent adopted by the primary ball milling is water, and the ball milling medium is zirconium balls;

(2) calcining the mixture obtained in the step (1) at 1000 ℃ for 5 hours in an oxygen atmosphere with the oxygen concentration of 90 vol% and the absolute pressure of 0.3MPa to obtain a pre-calcined material;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material with the average particle size of 8 microns; the dispersant adopted by the secondary ball milling is water, and the ball milling medium is zirconium balls;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder with the average particle size of 30 microns; the binder is polyvinyl alcohol aqueous solution, and the addition amount of the binder is 0.6 wt% of the ferrite powder;

(5) and (4) applying cold isostatic pressing with the pressure of 150MPa to the ferrite powder obtained in the step (4), and sintering at 1400 ℃ for 5 hours to obtain the ferrite material.

Example 2

This example provides a ferrite material suitable for miniaturized microwave devices, and the chemical formula of the ferrite material is Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.5, b is 0.1, c is 0.1, d is 0.2, and e is 0.1. The preparation method comprises the following steps:

(1) carrying out primary ball milling and mixing Y according to the formula amount₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃To obtain a mixture with the average grain diameter of 3 mu m; the dispersing agent adopted by the primary ball milling is absolute ethyl alcohol, and the ball milling medium is steel balls;

(2) calcining the mixture obtained in the step (1) at 900 ℃ for 6 hours in an oxygen atmosphere with the oxygen concentration of 80 vol% and the absolute pressure of 0.1MPa to obtain a pre-calcined material;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material with the average particle size of 5 microns; the dispersant adopted by the secondary ball milling is absolute ethyl alcohol, and the ball milling medium is steel balls;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder with the average particle size of 20 microns; the binder is carboxymethyl cellulose, and the addition amount of the binder is 0.4 wt% of the ferrite powder;

(5) and (4) applying cold isostatic pressing with the pressure of 100MPa to the ferrite powder obtained in the step (4), and sintering at 1300 ℃ for 6 hours to obtain the ferrite material.

Example 3

This example provides a ferrite material suitable for miniaturized microwave devices, and the chemical formula of the ferrite material is Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where, a is 1, b is 0.2, c is 0.2, d is 0.4, and e is 0.2. The preparation method comprises the following steps:

(1) carrying out primary ball milling and mixing Y according to the formula amount₂O₃、CaCO₃、TiO₂、ZrO₂、SnO₂、GeO₂With Fe₂O₃To obtain a mixture with the average grain diameter of 5 mu m; the dispersing agent adopted by the primary ball milling is water, and the ball milling medium is zirconium balls;

(2) calcining the mixture obtained in the step (1) at 1100 ℃ for 4h in an oxygen atmosphere with the oxygen concentration of 100 vol% and the absolute pressure of 0.5MPa to obtain a pre-calcined material;

(3) performing secondary ball milling on the pre-sintered material obtained in the step (2) to obtain a ball grinding material with the average particle size of 10 microns; the dispersant adopted by the secondary ball milling is water, and the ball milling medium is zirconium balls;

(4) mixing a binder with the ball grinding material obtained in the step (3), and performing spray granulation to obtain ferrite powder with the average particle size of 40 mu m; the binder is polyvinyl alcohol aqueous solution, and the addition amount of the binder is 0.8 wt% of the ferrite powder;

(5) and (4) applying cold isostatic pressing with the pressure of 200MPa to the ferrite powder obtained in the step (4), and sintering at 1500 ℃ for 4h to obtain the ferrite material.

Example 4

This example provides a ferrite material suitable for miniaturized microwave devices, and the chemical formula of the ferrite material is Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where, a is 1, b is 0.3, c is 0.2, d is 0.4, and e is 0.1. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Example 5

This example provides a ferrite material suitable for miniaturized microwave devices, and the chemical formula of the ferrite material is Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where, a is 1, b is 0.1, c is 0.4, d is 0.4, and e is 0.1. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 1

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 1.3, b is 0.3, c is 0.4, d is 0.4, and e is 0.2. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 2

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.4, b is 0.1, c is 0.1, d is 0.1, and e is 0.1. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 3

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.7, b is 0, c is 0.25, d is 0.3, and e is 0.15. The preparation method comprises the steps of adaptively adjusting the formula amount in the step (1) according to the composition chemical formula, and preparing the final productThe components are the same as those in embodiment 1, and thus are not described herein.

Comparative example 4

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.65, b is 0.2, c is 0, d is 0.3, and e is 0.15. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 5

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.6, b is 0.2, c is 0.25, d is 0, and e is 0.15. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 6

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Wherein a is 0.75, b is 0.2, c is 0.25, d is 0.3, and e is 0. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 7

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.35, b is 0.2, c is 0, and e is 0.15. The preparation method is characterized in that the formula amount in the step (1) is determined according to the compositionThe chemical formula is adjusted adaptively, and the rest conditions are the same as those in example 1, so that the details are not repeated herein.

Comparative example 8

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Wherein, a is 0.45, b is 0.2, c is 0.25, and d is 0. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 9

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.5, b is 0.2, c is 0, and d is 0.3. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 10

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Wherein, a-b-0.2, c-d-e-0. Except that the formula amount in the step (1) is adaptively adjusted according to the chemical formula of the composition, the other conditions are the same as those in the example 1, and thus the details are not repeated herein.

Comparative example 11

The present comparative example provides a ferrite material having a chemical formula of Y and a method for preparing the same_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂Where a is 0.9, b is 0.2, c is 0.25, d is 0.3, and e is 0.15. The preparation method is characterized in that oxygen in the step (2) is usedThe atmosphere was changed to nitrogen, and the rest of the conditions were the same as in example 1, and therefore, the details are not repeated herein.

The ferrite materials obtained in examples 1 to 5 and comparative examples 1 to 11 were tested for Curie temperature, saturation magnetization (25 ℃), dielectric constant, and ferromagnetic resonance line width. Measuring Curie temperature and saturation magnetization by using a vibrating sample magnetometer; testing the dielectric constant according to the IEC60556 standard, wherein the testing frequency is 10.7GHz, and the sample size is 1.6 mm; testing the ferromagnetic resonance line width according to the GB/T9633-88 standard; the final results are shown in table 1.

TABLE 1

	Saturation magnetization (Gs)	Dielectric constant	Curie temperature (. degree. C.)	Resonance line width (Oe)
					Example 1	1890	28	276	20
Example 2	1884	25	278	22
					Example 3	1895	26	268	24
Example 4	1680	21	264	30
					Example 5	1704	20	250	28
Comparative example 1	1679	18	262	26
					Comparative example 2	1710	22	255	32
Comparative example 3	1662	16	246	29
					Comparative example 4	1668	20	256	31
Comparative example 5	1660	22	260	34
					Comparative example 6	1712	21	245	32
Comparative example 7	1688	22	255	36
					Comparative example 8	1694	16	261	40
Comparative example 9	1687	14	260	37
					Comparative example 10	1682	20	238	38
Comparative example 11	1647	15	236	34

Thus, the invention provides a composition with the chemical formula of Y_3-aCa_aTi_bZr_cSn_dGe_eFe_5-b-c-d-eO₁₂The ferrite material is garnet type ferrite material Y₃Fe₅O₁₂Prepared on the basis of Ti by means of ion exchange⁴⁺、Zr⁴⁺、Sn⁴⁺With Ge⁴⁺In synergy, by partial substitution of Fe³⁺The ferromagnetic resonance line width of the obtained ferrite material is reduced, and the problem of overlarge ferromagnetic resonance line width caused by the addition of Bi is avoided; ca²⁺By partial substitution of Y³⁺The dielectric constant of the obtained ferrite material is improved, so that the obtained ferrite material has higher saturation magnetization, and the electromagnetic loss of the ferrite material when applied to a miniaturized microwave device is reduced; in addition, the preparation method provided by the invention prepares the pre-sintered material by carrying out oxygenation calcination on the mixed material, and Fe²⁺Is oxidized into Fe³⁺Inhibit Fe²⁺The generation of the ferrite reduces the super exchange effect strength in the obtained ferrite material, reduces the ferromagnetic resonance line width, improves the resistivity and reduces the dielectric loss; the dielectric constant of the ferrite material obtained by the invention is not lower than 20, the ferromagnetic resonance line width is not more than 30Oe, the Curie temperature can reach more than 250 ℃, the saturation magnetization can reach more than 1680Gs, and the ferrite material is particularly suitable for miniaturized microwave devices.

The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.