CN114436635A - Microwave ferrite material with high spin wave line width and preparation method thereof - Google Patents
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Abstract
The invention discloses a microwave ferrite material with high spin wave line width, belonging to the field of microwave ferrite materials, and the microwave ferrite material comprises the following chemical formula: y is3‑a‑bCaaGdbFe5‑c‑d‑e‑f‑g‑δZrcSndVeInfHfgO12Wherein a is more than or equal to 0 and less than or equal to 0.7, b is more than or equal to 0 and less than or equal to 0.7, c is more than or equal to 0 and less than or equal to 0.6, d is more than or equal to 0 and less than or equal to 0.7, e is more than or equal to 0 and less than or equal to 0.7, f is more than or equal to 0 and less than or equal to 0.3, and delta is the iron deficiencyThe microwave dielectric ceramic is used in power type microwave devices, and is particularly suitable for the fields of radar communication and the like.
Description
Technical Field
The invention relates to the field of microwave ferrite materials, in particular to a microwave ferrite material with high spin wave line width and a preparation method thereof.
Background
Microwave ferrite materials have many performance parameters, such as: saturation magnetization, ferromagnetic resonance linewidth, curie temperature, spin linewidth, temperature stability, and the like. Depending on the application environment of ferrite devices, different performance parameters are pursued, such as: in 4/5G communication, in order to pursue low loss and high bandwidth of devices, the microwave ferrite is mainly selected from garnet materials with low ferromagnetic resonance line width and high saturation magnetization; in the application scene of a wide temperature range, the material is required to have a low ferromagnetic resonance line width and a low temperature coefficient; in the application of satellite-borne high power, the device needs the microwave ferrite material to bear larger power, which requires the spin wave line width of the material to be larger. At present, Dy is the main means for improving the spin linewidth of materials in the garnet system3+、Tb3+、Ho3+The material grains are doped or refined by plasma, but the spin wave line width is improved by refining the grains, so that the application in specific engineering is less.
Disclosure of Invention
It is an object of the present invention to provide a microwave ferrite material with a high spin linewidth to solve the above problems.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a microwave ferrite material with high spin linewidth comprises the following chemical formula:
Y3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12wherein a is more than or equal to 0 and less than or equal to 0.7, b is more than or equal to 0 and less than or equal to 0.7, c is more than or equal to 0 and less than or equal to 0.6, d is more than or equal to 0 and less than or equal to 0.7, e is more than or equal to 0 and less than or equal to 0.7, f is more than or equal to 0 and less than or equal to 0.7, g is more than 0 and less than or equal to 0.3, and delta is the iron-deficiency.
The ferrite material of the present invention is prepared by adding Fe3+Position doping of a suitable amount of Hf4+The method can obviously improve the spin wave line width of the material, can be widely applied to the formula design for improving the spin wave line width of the microwave ferrite material, and enriches the technical means for regulating and controlling the spin wave line width.
The invention is formed by doping Hf4+The spin wave line width of the material is regulated and controlled, and the traditional Dy is changed3+、Tb3+、Ho3+Plasma substitution, or by refining the grains to increase the spin wave line width.
The second purpose of the present invention is to provide a method for preparing the above material, which adopts the technical scheme that the method comprises the following steps:
(1) preparing a primary material: weighing the raw materials according to the content of the chemical formula components, adding a solvent for ball milling for 4-12 h, filtering, drying, sieving, pre-sintering at 1280 ℃ at 1200-;
(2) preparing a secondary material: crushing the primary material obtained in the step (1), adding a solvent, ball-milling for 4-12 h, filtering and drying to obtain a secondary material;
(3) and (3) granulation: adding a certain amount of adhesive into the prepared secondary material, granulating and sieving;
(4) molding: putting the fine powder after granulation into a mould for pressing, wherein the pressing pressure is 50MPa to 250MPa, and obtaining a material green body
(5) Sintering; and (4) putting the green body into an air atmosphere or oxidizing atmosphere furnace for sintering to obtain a sample.
As a preferred technical scheme: the raw material in step (a) is analytically pure and has a chemical formula of Fe2O3、Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3。
As a preferred technical scheme: in the step (1), the ball-material ratio is 4:0.6, and the ball milling time is 4 h.
As a preferred technical scheme: in the step (1), the ball is zirconia, and the solvent is deionized water or alcohol.
As a preferable technical scheme: in the step (2), the ratio of the material to the solvent is 1:0.6, and the ball milling time is 4 h.
The size of the sieve in the step (1) and the step (3) is 20-60 meshes.
As a preferred technical scheme: in the step (3), the adhesive is a polyvinyl alcohol aqueous solution, and the concentration is 5-12 wt%.
As a preferred technical scheme: in the step (5), the sintering temperature is 1350-1450 ℃, and the temperature is kept for more than 6 hours.
Compared with the prior art, the invention has the following obvious differences:
the elements doped are different: dy is doped in the prior art for improving the spin linewidth of garnet materials3+、 Tb3+、Ho3+Plasma, and the present invention is disclosed for the first time in Fe3+Bit-doped Hf4+The spin linewidth of the garnet gyromagnetic material can also be obviously improved;
the position of doping is different: in the prior art, the spin wave line width of the garnet material is improved by doping at a Y position, but the spin wave line width of the garnet material is improved by doping at an Fe position, which has never been reported in previous researches.
Compared with the prior art, the invention has the advantages that: the technology of the invention can effectively regulate and control the spin wave line width and the ferromagnetic resonance line width of the microwave ferrite material, can enable the microwave ferrite material to meet devices with different power capacities of small, medium and high, can be widely applied to power type microwave devices, and is particularly suitable for the fields of radar communication and the like.
Detailed Description
The present invention will be further explained below.
Example 1: according to the formula3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12Weighing Fe2O3、 Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3Where a is 0.3, b is 0, c is 0, d is 0.2, e is 0, f is 0.1, g is 0.05, and δ is 0.05.
Example 2: according to the formula3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12Weighing Fe2O3、 Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3Where a is 0.3, b is 0, c is 0, d is 0.2, e is 0, f is 0.1, g is 0.1, and δ is 0.05.
Example 3: according to the formula3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12Weighing Fe2O3、 Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3Where a is 0.3, b is 0, c is 0, d is 0.2, e is 0, f is 0.1, g is 0.15, and δ is 0.05.
Example 4: according to the formula3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12Weighing Fe2O3、 Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3Where a is 0.3, b is 0, c is 0, d is 0.2, e is 0, f is 0.1, g is 0.2, and δ is 0.05.
Example 5: according to the formula3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12Weighing Fe2O3、 Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3Where a is 0.25, b is 0.4, c is 0.1, d is 0.1, e is 0.05, f is 0, g is 0.05, and δ is 0.05.
Example 6: pressing into a prescriptionChemical composition Y3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12Weighing Fe2O3、 Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3Where a is 0.25, b is 0.4, c is 0.1, d is 0.1, e is 0.05, f is 0, g is 0.1, and δ is 0.05.
The preparation method comprises the following steps: weighing the raw materials according to the embodiment 1-6, wherein the raw materials are all analytically pure;
preparing a primary material: carrying out wet ball milling on the weighed raw materials, and ball milling: material preparation: the proportion of the diluent is 4:1:1, (the ball is zirconia, the diluent is deionized water or alcohol), ball milling is carried out for 4 hours by a wet method, then filtering, drying and sieving are carried out, presintering treatment is carried out at 1260 ℃, and then natural cooling is carried out;
preparing a secondary material: and (3) smashing the prepared primary particles, pouring the smashed primary particles into a ball milling tank, and carrying out secondary ball milling, wherein the ball: material preparation: the proportion of the diluent is 4:1:0.6, the wet ball milling is carried out for 4 hours, and then the filtration and the drying are carried out;
and (3) granulation: adding the secondary material into 9 wt% polyvinyl alcohol aqueous solution, fully mixing and sieving;
molding: placing the granulated particles into a die for pressing, wherein the pressing pressure is 100MPa, and obtaining a material green body;
and (3) sintering: placing the green body into an air atmosphere furnace for sintering, wherein the sintering temperature is 1400 ℃, and naturally cooling after the heat preservation time is 8 hours;
and (3) testing: the sintered sample is subjected to performance tests, and the test results of density, saturation magnetization, ferromagnetic resonance line width and spin wave line width are shown in table 1;
TABLE 1 Properties of ferrites of examples 1-4
Analyzing the performance data:
comparative examples 1 to 4: with the increase of Hf element, the spin wave line width and the ferromagnetic resonance line width are obviously increased; the embodiments 1, 2 and 3 of the invention realize better microwave performance, and simultaneously give consideration to the requirements of engineering on the ferromagnetic resonance line width and the spin wave line width of the material.
Comparative examples 5, 6: the line widths of the ferromagnetic resonance and spin wave have the same variation tendency as those of examples 1 to 4.
Compared with the prior art, the invention has the following obvious differences:
the elements doped are different: dy is doped in the prior art for improving the spin linewidth of garnet materials3+、 Tb3+、Ho3+Plasma, and the present invention is disclosed for the first time in Fe3+Bit-doped Hf4+The spin linewidth of the garnet gyromagnetic material can also be obviously improved;
the position of doping is different: in the prior art, the spin wave line width of the garnet material is improved by doping at a Y position, but the spin wave line width of the garnet material is improved by doping at an Fe position, which has never been reported in previous researches.
The technology of the invention can effectively regulate and control the spin wave line width and the ferromagnetic resonance line width of the microwave ferrite material, can enable the microwave ferrite material to meet devices with different power capacities of small, medium and high, can be widely applied to power type microwave devices, and is particularly suitable for the fields of radar communication and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A microwave ferrite material having a high spin linewidth, characterized by: the chemical formula of the compound is as follows:
Y3-a-bCaaGdbFe5-c-d-e-f-g-δZrcSndVeInfHfgO12whereinA is more than or equal to 0 and less than or equal to 0.7, b is more than or equal to 0 and less than or equal to 0.7, c is more than or equal to 0 and less than or equal to 0.6, d is more than or equal to 0 and less than or equal to 0.7, e is more than or equal to 0 and less than or equal to 0.7, f is more than or equal to 0 and less than or equal to 0.7, g is more than 0 and less than or equal to 0.3, and delta is the iron-deficiency.
2. The method for preparing a microwave ferrite material with high spin linewidth of claim 1, comprising the steps of:
(1) preparing a primary material: weighing the raw materials according to the content of the main components, adding a solvent for ball milling for 4-12 h, filtering, drying, sieving, pre-sintering at 1280 ℃ under 1200-;
(2) preparing a secondary material: crushing the primary material obtained in the step (1), adding a solvent, ball-milling for 4-12 h, filtering and drying to obtain a secondary material;
(3) and (3) granulation: adding the prepared secondary material into an adhesive, granulating and sieving;
(4) molding: putting the granulated fine powder into a die for pressing, wherein the pressing pressure is 50-250 MPa, and obtaining a material green body;
(5) sintering; and (3) putting the green body into an air atmosphere or oxidizing atmosphere furnace for sintering to obtain the ceramic material.
3. The method of claim 2, wherein: the raw material in step (a) is analytically pure and has a chemical formula of Fe2O3、Gd2O3、CaCO3、ZrO2、SnO2、V2O5、In2O3、HfO2、Y2O3。
4. The method of claim 2, wherein: in the step (1), the ball-material ratio is 4:0.6 during ball milling, and the ball milling time is 4 h.
5. The method of claim 2, wherein: in the step (1), the ball is zirconia during ball milling, and the solvent is deionized water or alcohol.
6. The method of claim 2, wherein: in the step (2), the ratio of the material to the solvent is 1:0.6, and the ball milling time is 4 h.
7. The method of claim 2, wherein: the size of the sieve during sieving in the steps (1) and (3) is 20-60 meshes.
8. The method of claim 2, wherein: in the step (3), the adhesive is a polyvinyl alcohol aqueous solution, and the concentration is 5-12 wt%.
9. The method of claim 2, wherein: in the step (5), the sintering temperature is 1350-1450 ℃, and the temperature is kept for more than 6 hours.
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| CN106220158A (en) * | 2016-08-03 | 2016-12-14 | 中国航天时代电子公司 | A kind of High-Power Microwave Ferrite Material and preparation method thereof |
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