A preparation method of a gyromagnetic ferrite material applied to a high-power microwave device

By mixing and treating Fe2O3, Y2O3, Bi2O3, CaO, and ZrO2 materials in specific proportions, and using citric acid and polyvinyl alcohol solutions, the problem of uneven internal composition of gyromagnetic ferrite materials was solved, thereby improving electromagnetic properties and the overall quality of the materials.

CN119751039BActive Publication Date: 2026-01-02NANJING BIAO ELECTRONIC TECH CO LTD
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Patent Information

Application Number
CN202411707442.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-27
Publication Date
2026-01-02
Estimated Expiration
2044-11-27

AI Technical Summary

Technical Problem

In the prior art, the prepared gyromagnetic ferrite materials have poor diffusion during powder mixing and sintering, resulting in uneven internal component distribution and poor electromagnetic properties.

Method used

Fe2O3, Y2O3, Bi2O3, CaO, and ZrO2 are mixed in a specific ratio, ball-milled and dried, sieved, mixed with citric acid, and calcined by stepwise heating. After being pulverized and ball-milled, polyvinyl alcohol solution is added for granulation. The green body is sintered and annealed under specific conditions to form a ferromagnetic ferrite material with uniform internal composition.

Benefits of technology

This improved the electromagnetic properties of the gyromagnetic ferrite material, reduced the ferromagnetic resonance linewidth, decreased magnetic loss, and enhanced the overall performance of the material.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to the technical field of electronic ceramic materials, in particular to a preparation method of a gyromagnetic ferrite material applied to a high-power microwave device. The preparation method comprises the following steps: firstly, dry Fe2O3, Y2O3, Bi2O3, CaO and ZrO2 are mixed according to specific proportions, then the mixture is added into anhydrous ethanol, and the mixture is dried after ball milling, and the mixture is screened through a screen with a specific aperture size to obtain a raw material composition; secondly, the raw material composition and citric acid are uniformly mixed according to specific proportions, and then the mixture is loaded into an alumina sealing tank, the tank is sealed, and the mixture is subjected to step-by-step temperature rising calcination, then the mixture is crushed and ball milled, and the mixture is dried again, and the mixture is screened through the screen with the specific aperture size to obtain a pre-sintering composition; thirdly, polyvinyl alcohol solution is added into the pre-sintering composition, the mixture is stirred uniformly, granulation is carried out, and the mixture is compressed into a green body; finally, the green body is subjected to sintering and re-sintering, and then the green body is subjected to annealing under a specific oxygen flow to obtain the gyromagnetic ferrite material which has a uniform internal composition distribution, better electromagnetic performance and a wide application prospect.
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Description

TECHNICAL FIELD

[0001] The application relates to the technical field of electronic ceramic materials, in particular to a preparation method of gyromagnetic ferrite material applied to a high-power microwave device. BACKGROUND

[0002] Ferrite is a non-metallic magnetic material, which is usually a composite oxide of iron and other metal elements. The resistivity of the ferrite can reach 102-1011 ohm*cm. In terms of dielectric performance, the dielectric constant is generally 8-16, and the dielectric loss tangent can reach 10 -3 -10 -4 The saturation magnetization is generally 200-5500 Gauss, and the Curie temperature is generally within the range of 100-600 DEG C. According to the crystal structure, the ferrite can be divided into three types: spinel type, garnet type and magnetoplumbite type. According to the characteristics and uses of the ferrite, the ferrite can be divided into five categories: soft magnetic ferrite, hard magnetic ferrite, gyromagnetic ferrite, square magnetic ferrite and piezomagnetic ferrite. The gyromagnetic ferrite material is different from other soft magnetic, hard magnetic and other ferrite materials. The other several magnetic materials generally work by using the magnetic characteristics. The gyromagnetic ferrite material itself does not show magnetism. Under the action of an external magnetic field, the gyromagnetic material shows the characteristics of tensor permeability, ferromagnetic resonance, Faraday rotation and field shift effect on a microwave signal. By using the characteristics, various microwave magnetic devices with excellent performance can be made, such as isolators, circulators, electrically controlled phase shifters, electrically controlled switches, polarization converters, electrically tunable filters, oscillators and delay lines. The garnet-type gyromagnetic ferrite material is one of the indispensable magnetic materials in domestic and foreign military and civil electronic equipment at present and in a long period of time in the future. The garnet-type gyromagnetic ferrite material has excellent performance such as low loss, high resistivity and narrow resonance line width in the microwave frequency band, and has extremely high application value.

[0003] The circulators and isolators in microwave devices work in the general range of -55℃ to 85℃, which requires that the gyromagnetic ferrite material used by the circulators and isolators can maintain good performance in a wide temperature range. In practical applications, there are many garnet-type gyromagnetic ferrite materials, and the saturation magnetization of these materials changes greatly with temperature. In particular, in high-power microwave devices, not only does the change in ambient temperature affect the saturation magnetization of the ferrite, but also the self-heating of the ferrite material is greater due to the high operating power of the device. In addition, the ferrite substrate is located near the center of the microwave device, and its heat dissipation rate is slower than that of the external magnetic field, so the temperature of the ferrite itself is higher than that of the external magnetic field. The change in the saturation magnetization of the ferrite material is always greater than the change in the strength of the external magnetic field. At this time, the saturation magnetization of the ferrite substrate in the circulator and isolator will change greatly, thereby degrading the performance of the circulator and isolator.

[0004] To solve this problem, patent technical document CN115331907B discloses a preparation method of a gyromagnetic ferrite material applied to a high-power microwave device. Fe2O3, Y2O3, Gd2O3, Dy2O3, V2O5, ZrO2, Al(OH)3, CaCO3, and MnCO3 are used as raw materials, and the mass ratio of each raw material is calculated according to the chemical formula. The weighed raw materials are loaded into a stainless steel ball mill jar, an appropriate amount of steel balls and anhydrous ethanol are added, the ball mill jar is sealed, and ball milling is performed. After the mixed raw materials are ball milled once, the anhydrous ethanol is dried, the mixed raw materials are pressed into a round cake, and the round cake is placed in a high-temperature electric furnace for pre-burning. The pre-burned mixed material is crushed and loaded into a stainless steel ball mill jar, an appropriate amount of steel balls and anhydrous ethanol are added, the jar is sealed, and ball milling is performed. The mixed powder after the second ball milling is dried, polyvinyl alcohol solution is added for granulation, and the green body is pressed. The green body is placed in a high-temperature electric furnace for oxygen sintering.

[0005] However, these existing preparation methods still have the problem that the gyromagnetic ferrite material prepared has poor diffusion during powder mixing and sintering, resulting in uneven distribution of internal components and poor electromagnetic performance of the material.

[0006] Therefore, according to the related technology in the above, it is urgent to develop a preparation method of a gyromagnetic ferrite material applied to a high-power microwave device. SUMMARY

[0007] Therefore, according to the related technology in the above, it is urgent to develop a preparation method of a gyromagnetic ferrite material applied to a high-power microwave device.

[0008] Based on the above purpose, the application provides a preparation method of a gyromagnetic ferrite material applied to a high-power microwave device.

[0009] A preparation method of a gyromagnetic ferrite material applied to a high-power microwave device, the preparation method is as follows:

[0010] Step S1. Dry Fe2O3, Y2O3, Bi2O3, CaO, ZrO2 are mixed and then added with anhydrous ethanol, ball-milled at 800-1000 rpm for 8-10 h, dried at 120-130 ℃, and then sieved to obtain a raw material composition;

[0011] Step S2. The raw material composition and citric acid are uniformly mixed and then loaded into an alumina sealed tank, and then subjected to step-by-step temperature rising calcination after sealing, followed by crushing and ball-milling at 300-500 rpm for 24-25 h, and then dried at 120-130 ℃ and sieved again to obtain a pre-sintered composition;

[0012] Step S3. Polyvinyl alcohol solution is added to the pre-sintered composition, stirred at 800-1000 rpm for 1-3 h, and then granulated, and then compressed into a green body;

[0013] Step S4. The green body is sintered and then re-sintered, and then annealed under the condition that the oxygen flow is 200-210 mL / min for 2-2.5 h to obtain a gyromagnetic ferrite material applied to a high-power microwave device.

[0014] Preferably, the mass ratio of Fe2O3, Y2O3, Bi2O3, CaO, ZrO2 and anhydrous ethanol in step S1 is 79-79.85:66-67.74:9.32-11.65:0.56-0.95:1.23-3.7:35-40.

[0015] Preferably, the size of the mesh aperture in the sieving in step S1 is 30-38 μm.

[0016] Preferably, the mass ratio of the raw material composition and citric acid in step S2 is 155-160:10-15.

[0017] Preferably, the step-by-step temperature rising calcination process in step S2 is as follows:

[0018] The sealed alumina sealed tank is first calcined at 400-600 ℃ for 1-2 h, then calcined at 600-800 ℃ for 1-2 h, and then calcined at 800-850 ℃ for 6-8 h.

[0019] Preferably, the size of the mesh aperture in the sieving in step S2 is 0.15-0.3 mm.

[0020] Preferably, the mass ratio of the pre-sintering composition and the polyvinyl alcohol solution in step S3 is 150-155:15-18.

[0021] Preferably, the concentration of the polyvinyl alcohol solution in step S3 is 5wt%-5.2wt%.

[0022] Preferably, the sintering temperature in step S4 is 870-890℃, the gas pressure is 8-8.5MPa, and the sintering time is 5-6h.

[0023] Preferably, the re-sintering temperature in step S4 is 890-940℃, the gas pressure is 7-16MPa, and the sintering time is 1-2h.

[0024] Advantages of the present application:

[0025] The present application provides a preparation method of gyromagnetic ferrite material applied to high-power microwave devices. In the preparation method, dry Fe2O3, Y2O3, Bi2O3, CaO and ZrO2 are mixed according to specific proportions, then added with anhydrous ethanol, ball milled, dried, sieved with a sieve with a specific aperture size to obtain a raw material composition. Then, the raw material composition and citric acid are mixed according to specific proportions, then loaded into an alumina sealed tank, sealed, and subjected to step-by-step temperature rising calcination. After crushing and ball milling, the mixture is dried again, then sieved with a sieve with a specific aperture size to obtain a pre-sintering composition. Then, polyvinyl alcohol solution is added to the pre-sintering composition and stirred uniformly, then granulated and compressed into a green body. After sintering and re-sintering, the green body is annealed under a specific oxygen flow to obtain a gyromagnetic ferrite material with uniform internal composition distribution, better electromagnetic properties and wide application prospects. DETAILED DESCRIPTION

[0026] To make the purpose, technical solutions and advantages of the present application clearer, the present application is further described in detail below with specific examples.

[0027] The sources and properties of some raw materials used in the present application are as follows:

[0028] Fe2O3 is purchased from Zhejiang Yamei Nanometer Technology Co., Ltd., CAS: 1309-37-1; Y2O3 is purchased from Yumu (Ningbo) New Material Co., Ltd., CAS: 1314-37-0; Bi2O3 is purchased from Yumu (Ningbo) New Material Co., Ltd., CAS: 1304-76-3; CaO is purchased from Hubei Widelichemical Technology Co., Ltd., CAS: 1305-78-8; ZrO2 is purchased from Yumu (Ningbo) New Material Co., Ltd., CAS: 1314-23-4; citric acid is purchased from Jiangsu Weizhinrun Biological Technology Co., Ltd., CAS: 77-92-7.

[0029] Example 1: A preparation method of a gyromagnetic ferrite material applied to a high-power microwave device is as follows:

[0030] S1. After mixing 79g of dried Fe2O3, 66g of Y2O3, 9.32g of Bi2O3, 0.56g of CaO, and 1.23g of ZrO2, 35g of anhydrous ethanol is added, and ball milling is performed at 800 rpm for 8h. After drying at 120℃, the raw material composition is obtained by sieving with a sieve having a mesh size of 30μm;

[0031] S2. After uniformly mixing 155g of the raw material composition and 10g of citric acid, the mixture is loaded into an alumina sealed tank. After sealing, calcination is performed at 400℃ for 1h, then at 600℃ for 1h, and then at 800℃ for 6h. After crushing and ball milling at 300 rpm for 24h, the presintered composition is obtained by sieving again with a sieve having a mesh size of 0.15mm after drying at 120℃;

[0032] Step S3. After adding 15g of a polyvinyl alcohol solution having a concentration of 5wt% to 150g of the presintered composition, stirring is performed at 800 rpm for 1h, and then granulation is performed. The granulated product is compressed into a green body;

[0033] Step S4. After sintering the green body at 870℃ and 8MPa for 5h, and then resintering at 890℃ and 7MPa for 1h, the gyromagnetic ferrite material applied to the high-power microwave device is obtained by annealing in an oxygen flow of 200mL / min for 2h;

[0034] Example 2: A preparation method of a gyromagnetic ferrite material applied to a high-power microwave device is as follows:

[0035] S1. After mixing 79.3g of dried Fe2O3, 66.54g of Y2O3, 10g of Bi2O3, 0.67g of CaO, and 1.9g of ZrO2, 37g of anhydrous ethanol is added, and ball milling is performed at 880 rpm for 8.5h. After drying at 125℃, the raw material composition is obtained by sieving with a sieve having a mesh size of 35μm;

[0036] S2. After uniformly mixing 157g of the raw material composition and 12g of citric acid, the mixture is loaded into an alumina sealed tank. After sealing, calcination is performed at 480℃ for 1.2h, then at 680℃ for 1.4h, and then at 820℃ for 6.5h. After crushing and ball milling at 370 rpm for 24.5h, the presintered composition is obtained by sieving again with a sieve having a mesh size of 0.18mm after drying at 123℃;

[0037] S3. 16 g of a polyvinyl alcohol solution with a concentration of 5.1 wt% was added to 152 g of the pre-sintered composition, which was granulated after stirring at 880 rpm for 1.7 h, and then compressed into a green body;

[0038] S4. The green body was sintered at 877℃ under a pressure of 8.2 MPa for 5.3 h, and then re-sintered at 900℃ under a pressure of 10 MPa for 1.3 h, and then annealed under an oxygen flow of 203 mL / min for 2.2 h to obtain a gyromagnetic ferrite material for high-power microwave devices;

[0039] Example 3: A preparation method of a gyromagnetic ferrite material for high-power microwave devices is as follows:

[0040] S1. Dry 79.65 g of Fe2O3, 67.24 g of Y2O3, 11 g of Bi2O3, 0.8 g of CaO, and 2.5 g of ZrO2 were mixed, 38 g of anhydrous ethanol was added, and ball milling was performed at 920 rpm for 9.5 h, and then drying was performed at 127℃, and sieving was performed using a sieve with a pore size of 36 μm to obtain a raw material composition;

[0041] S2. 158 g of the raw material composition and 14 g of citric acid were mixed and uniformly mixed, and then placed in an alumina sealed tank, and after sealing, calcination was first performed at 530℃ for 1.8 h, and then calcination was performed at 730℃ for 1.7 h, and then calcination was performed at 840℃ for 7.5 h, and then the powder was crushed and ball milling was performed at 430 rpm for 24.7 h, and then drying was performed at 127℃, and sieving was again performed using a sieve with a pore size of 0.21 mm to obtain a pre-sintered composition;

[0042] S3. 17 g of a polyvinyl alcohol solution with a concentration of 5.1 wt% was added to 154 g of the pre-sintered composition, which was granulated after stirring at 950 rpm for 1.7 h, and then compressed into a green body;

[0043] S4. The green body was sintered at 885℃ under a pressure of 8.4 MPa for 5.6 h, and then re-sintered at 920℃ under a pressure of 15.5 MPa for 1.7 h, and then annealed under an oxygen flow of 205 mL / min for 2.3 h to obtain a gyromagnetic ferrite material for high-power microwave devices;

[0044] Example 4: A preparation method of a gyromagnetic ferrite material for high-power microwave devices is as follows:

[0045] S1. Mix 79.85 g of Fe2O3, 67.74 g of Y2O3, 11.65 g of Bi2O3, 0.95 g of CaO, 3.7 g of ZrO2, and then add 40 g of anhydrous ethanol, ball mill at 1000 rpm for 10 h, dry at 130°C, sieve with a sieve screen with a pore size of 30-38 μm to obtain a raw material composition;

[0046] S2. Mix 160 g of the raw material composition and 15 g of citric acid, and then put into an alumina sealed tank, seal, first calcine at 600°C for 2 h, then calcine at 800°C for 2 h, and then calcine at 850°C for 8 h, then crush and ball mill at 500 rpm for 25 h, dry at 130°C, and sieve again with a sieve screen with a pore size of 0.3 mm to obtain a pre-sintered composition;

[0047] S3. Add 18 g of a polyvinyl alcohol solution with a concentration of 5.2 wt% to 155 g of the pre-sintered composition, stir at 1000 rpm for 3 h, then granulate, and then compress into a green body;

[0048] S4. Sinter the green body at 890°C and 8.5 MPa for 6 h, then re-sinter at 940°C and 16 MPa for 2 h, and then anneal at an oxygen flow rate of 210 mL / min for 2.5 h to obtain a gyromagnetic ferrite material for high-power microwave devices;

[0049] Comparative Example 1:

[0050] This comparative example is compared with Example 1 only by replacing “79 g of Fe2O3, 66 g of Y2O3, 9.32 g of Bi2O3, 0.56 g of CaO, 1.23 g of ZrO2” added in the raw material composition preparation process with “79 g of Fe2O3, 66 g of Y2O3, 3.32 g of Bi2O3, 3.56 g of CaO, 4.23 g of ZrO2”, and the rest of the steps and parameters are the same, which will not be repeated here. The final gyromagnetic ferrite material for high-power microwave devices is obtained;

[0051] Comparative Example 2:

[0052] This comparative example is compared with Example 1 only by replacing “a sieve screen with a pore size of 30 μm” used in the raw material composition preparation process with “a sieve screen with a pore size of 0.85 mm”, and the rest of the steps and parameters are the same, which will not be repeated here. The final gyromagnetic ferrite material for high-power microwave devices is obtained;

[0053] Comparative Example 3

[0054] The comparative example is compared with example 1, no citric acid is added in the preparation process of the pre-sintering composition, the remaining steps and parameters are the same, the comparative example will not be repeated, and finally the gyromagnetic ferrite material applied to the high-power microwave device is obtained;

[0055] Comparative example 4:

[0056] The comparative example is compared with example 1, only the “calcination at 400℃ for 1h after sealing, and then calcination at 600℃ for 1h, and then calcination at 800℃ for 6h” used in the preparation process of the pre-sintering composition is replaced by “calcination at 800℃ for 8h after sealing”, the remaining steps and parameters are the same, the comparative example will not be repeated, and finally the gyromagnetic ferrite material applied to the high-power microwave device is obtained;

[0057] Comparative example 5:

[0058] The comparative example is compared with example 1, only the “sieve screen with a pore size of 0.15mm” used in the preparation process of the pre-sintering composition is replaced by “sieve screen with a pore size of 0.85mm”, the remaining steps and parameters are the same, the comparative example will not be repeated, and finally the gyromagnetic ferrite material applied to the high-power microwave device is obtained;

[0059] Comparative example 6:

[0060] The comparative example is compared with example 1, only the “annealing for 2h under the condition of oxygen flow of 200mL / min” used in the preparation process of the gyromagnetic ferrite material applied to the high-power microwave device is replaced by “annealing for 2h under the condition of air flow of 200mL / min”, the remaining steps and parameters are the same, the comparative example will not be repeated, and finally the gyromagnetic ferrite material applied to the high-power microwave device is obtained;

[0061] Comparative example 7:

[0062] The comparative example is compared with example 1, only the “sintering of the green body at 870℃, 8MPa for 5h, and then re-sintering at 890℃, 7MPa for 1h” used in the preparation process of the gyromagnetic ferrite material applied to the high-power microwave device is replaced by “re-sintering of the green body at 890℃, 7MPa for 6h”, the remaining steps and parameters are the same, the comparative example will not be repeated, and finally the gyromagnetic ferrite material applied to the high-power microwave device is obtained;

[0063] Comparative example 8:

[0064] The comparative example is compared with example 1 only to replace the "sintering green body at 870 DEG C, 8 MPa for 5h, and then re-sintering at 890 DEG C, 7 MPa for 1h" used in the preparation process of the gyromagnetic ferrite material applied to the high-power microwave device with "sintering green body at 870 DEG C, 0 MPa for 5h, and then re-sintering at 890 DEG C, 0 MPa for 1h", and the rest of the steps and parameters are the same, which will not be repeated. The final gyromagnetic ferrite material applied to the high-power microwave device is obtained.

[0065] Performance test:

[0066] Saturated magnetization determination:

[0067] The saturated magnetization of the gyromagnetic ferrite material samples prepared in example 1-4 and comparative example 1-8 is determined by a vibrating sample magnetometer (Yingpu magnetoelectric technology development Co., Ltd. of Changchun, VSM-220);

[0068] Ferromagnetic resonance line width determination:

[0069] The gyromagnetic ferrite material samples prepared in example 1-4 and comparative example 1-8 are processed into 0.6mm diameter spheres, and then placed in a TE106 transmission type resonant cavity, the center frequency is set to 9.3GHz, and the ferromagnetic resonance line width of the gyromagnetic ferrite material prepared in example 1-4 and comparative example 1-8 is determined;

[0070] Dielectric constant determination:

[0071] The dielectric constant of the gyromagnetic ferrite material prepared in example 1-4 and comparative example 1-8 is determined by an impedance analyzer (Ernst instrument Co., Ltd., E4991B) at a frequency of 1MHz.

[0072] Table 1

[0073]

[0074]

[0075] Data analysis:

[0076] As can be seen from table 1, the saturated magnetization, ferromagnetic resonance line width and dielectric constant of the gyromagnetic ferrite material prepared by the present application are excellent, and these data show that the gyromagnetic ferrite material prepared by the present application has better electromagnetic performance;

[0077] The present application can provide the best calcined raw materials for the preparation of the pre-sintering composition, because the specific proportions of Fe2O3, Y2O3, Bi2O3, CaO and ZrO2 are added, and then the raw material composition is obtained after drying, ball milling and screening with a specific aperture size; the complex can be formed by mixing the treated raw material composition and citric acid in a specific proportion, so that the agglomeration of metal ions is reduced, and the metal ions are uniformly dispersed in the solution, which helps the components in the material to be more uniformly distributed in the subsequent sintering process, thereby improving the quality and performance of the ceramic; meanwhile, the citric acid will decompose and burn in the sintering process, and the generated gas can form pore channels in the ceramic material to promote the transmission and diffusion of substances, thereby reducing the temperature required for sintering, which not only can save energy and reduce production costs, but also can reduce the impact of high temperature on the structure and performance of the ceramic material; the components in the material can be further uniformly distributed by using the step-by-step heating calcination; then the pre-sintering composition can be obtained by crushing, ball milling, drying and screening with a specific aperture size, so that the components in the prepared green body are more uniformly dispersed; finally, the green body is sintered at a lower temperature and then re-sintered at a higher temperature, and the specific size of the air pressure is applied during the whole sintering process, and the annealing is performed under a specific oxygen flow, because compared with direct high-temperature sintering, the components in the material can be more uniformly distributed by first sintering at a suitable lower temperature and then re-sintering at a higher temperature, and the porosity of the sintered gyromagnetic ferrite material is also greatly reduced; compared with pressureless sintering, the porosity of the sample under hot-pressing sintering is significantly reduced, so that the obtained ferromagnetic resonance line width is also lower, and the overall electromagnetic performance of the prepared gyromagnetic ferrite material is also significantly improved, with lower ferromagnetic resonance line width, which means lower magnetic loss; compared with air annealing, the electromagnetic performance of the gyromagnetic ferrite material prepared by annealing under a specific oxygen flow is also improved; therefore, the internal component distribution of the prepared gyromagnetic ferrite material is uniform, and the electromagnetic performance is better.

[0078] It should be understood by those skilled in the art that the discussion of any embodiment is merely exemplary and is not intended to limit the scope of the application to these examples; under the idea of the present application, the technical features of the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other changes of different aspects of the present application as described above, which are not provided in detail for the sake of brevity.

[0079] The present application is intended to cover all such alternatives, modifications and variations as fall within the broad scope of the appended claims. Accordingly, any and all such alternatives, modifications and variations are intended to be encompassed by the appended claims.

Claims

1. A method for producing gyromagnetic ferrite material for use in high power microwave devices, characterized by, The preparation method is as follows: Step S1. After mixing dry Fe2O3, Y2O3, Bi2O3, CaO, ZrO2, add anhydrous ethanol, ball mill at 800-1000 rpm for 8-10 h, then dry at 120-130°C, sieve to obtain the raw material composition; Step S2. Mix the raw material composition and citric acid, then load into an alumina sealed tank, after sealing, perform step-by-step temperature rising calcination, then crush and ball mill at 300-500 rpm for 24-25 h, then dry at 120-130°C, sieve again to obtain the pre-sintered composition; Step S3. Add polyvinyl alcohol solution to the pre-sintered composition, stir at 800-1000 rpm for 1-3 h, then granulate, then compress into a green body; Step S4. After sintering and re-sintering, anneal under the condition of oxygen flow of 200-210 mL / min for 2-2.5 h to obtain the gyromagnetic ferrite material for high-power microwave devices; The mass ratio of Fe2O3, Y2O3, Bi2O3, CaO, ZrO2 and anhydrous ethanol in step S1 is 79-79.85:66-67.74:9.32-11.65:0.56-0.95:1.23-3.7:35-40; The sintering temperature in step S4 is 870-890°C, the gas pressure is 8-8.5 MPa, and the sintering time is 5-6 h; The re-sintering temperature in step S4 is 890-940°C, the gas pressure is 7-16 MPa, and the sintering time is 1-2 h.

2. The method of producing gyromagnetic ferrite material for use in high power microwave devices according to claim 1, characterized in that, The mesh size of the sieve in step S1 is 30-38 μm.

3. The method of producing gyromagnetic ferrite material for use in high power microwave devices according to claim 1, characterized in that, The mass ratio of the raw material composition and citric acid in step S2 is 155-160:10-15.

4. The method of producing gyromagnetic ferrite material for use in high power microwave devices according to claim 1, characterized in that, The step-by-step temperature rising calcination process in step S2 is as follows: First calcine the sealed alumina sealed tank at 400-600°C for 1-2 h, then at 600-800°C for 1-2 h, and then at 800-850°C for 6-8 h.

5. The method of producing gyromagnetic ferrite material for use in high power microwave devices according to claim 1, characterized in that, The mesh size of the sieve in step S2 is 0.15-0.3 mm.

6. The method of producing gyromagnetic ferrite material for use in high power microwave devices according to claim 1, characterized in that, The mass ratio of the pre-sintered composition and polyvinyl alcohol solution in step S3 is 150-155:15-18.

7. The method of producing gyromagnetic ferrite material for use in high power microwave devices according to claim 1, characterized in that, The concentration of the polyvinyl alcohol solution in step S3 is 5wt%-5.2wt%.

Citation Information

Patent Citations

  • A gyromagnetic ferrite material for high-power microwave devices and its preparation method

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