CN117700221A - Preparation method of coated high-dielectric low-loss microwave ferrite material - Google Patents
Preparation method of coated high-dielectric low-loss microwave ferrite material Download PDFInfo
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- CN117700221A CN117700221A CN202311757604.6A CN202311757604A CN117700221A CN 117700221 A CN117700221 A CN 117700221A CN 202311757604 A CN202311757604 A CN 202311757604A CN 117700221 A CN117700221 A CN 117700221A
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- 239000000463 material Substances 0.000 title claims abstract description 75
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
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- 238000000498 ball milling Methods 0.000 claims description 20
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- 239000008103 glucose Substances 0.000 claims description 14
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- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
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- 230000005350 ferromagnetic resonance Effects 0.000 abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 239000012776 electronic material Substances 0.000 abstract description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 12
- 229910000480 nickel oxide Inorganic materials 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 5
- 239000002223 garnet Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
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- 238000010438 heat treatment Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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Abstract
A preparation method of a coated high-dielectric low-loss microwave ferrite material belongs to the field of electronic materials. The coated high-dielectric low-loss microwave ferrite material provided by the invention has the advantages that the inner core NiCuZn ferrite is based on the NiCuZn ferrite material, the Ir element is adopted for performance regulation, the microwave loss of the material is reduced, and the excellent low-loss ferrite is obtained; the shell is a carbon sphere prepared by a hydrothermal method, has a good dielectric constant, is coated outside ferrite, and has good uniformity, so that the dielectric constant of the material is improved. The coated high-dielectric low-loss microwave ferrite material prepared by the invention has high dielectric constant (epsilon' =30-60) and low microwave loss (ferromagnetic resonance line width delta H=120-180 Oe) in a microwave frequency band (9.56 GHz), and meets the application requirements of circulators, isolators and phase shifters in the microwave frequency band.
Description
Technical Field
The invention belongs to the field of electronic materials, and particularly relates to a preparation method of a coated high-dielectric low-loss microwave ferrite material.
Background
With the rapid development of 5G/6G communication, information transmission in the microwave frequency band is becoming one of the main modes, and in a microwave transmission system, the size and performance of a microwave device directly affect the integration level and transmission characteristics of the whole microwave system. The performance of the devices is determined by the substrate material and the circuit design, especially the substrate material, and the area of the circuit design is firstly determined, and the performance of the substrate material directly influences the performance of the devices, such as the dielectric constant of the substrate material in the microwave devices, and directly influences the size of the devices, because in the microwave frequency band application, when electromagnetic waves propagate through the dielectric material, the wavelength is inversely proportional to the dielectric constant, which means that as the dielectric constant becomes larger, the wavelength becomes shorter, and the size of the microwave devices can be reduced; and secondly, the ferromagnetic resonance line width of the material influences the transmission efficiency of the microwave device, and the lower ferromagnetic resonance line width can enable the microwave device to have lower microwave loss in the application process, so that higher transmission efficiency is obtained. Therefore, the design and preparation of materials with high dielectric constant and low ferroresonance line width are one of the main research directions of microwave device materials.
Among the microwave ferrite materials, the garnet-type ferrite material, which is one of the excellent base materials of the microwave device by virtue of its excellent ferromagnetic resonance linewidth characteristics, has been the most studied. However, garnet-type ferrite materials generally have a dielectric constant of about 14 while possessing a relatively low ferroresonance linewidth. Various ion-modified garnet ferrite materials are adopted in the garnet type microwave ferrite sheet and the preparation method thereof (patent number ZL 202110883334.8), and the ferromagnetic resonance line width delta H is within 20, but the dielectric constant is not expressed. The garnet ferrite material has a dielectric constant of not less than 20, a ferromagnetic resonance line width of not more than 30Oe, and can be further improved in the aspect of device miniaturization although the dielectric constant is improved. The garnet ferrite material is modified by Bi, ca, zr, V and other elements to obtain a high dielectric constant (epsilon=23-25), the medium saturation magnetization material can be used for preparing a ferrite material with a ferromagnetic resonance linewidth lower than 300Oe, and the garnet ferrite material with a high dielectric constant and a low linewidth and the preparation method (application number: 202310391039. X) are modified by Bi, ca, zr, in and other elements to improve the dielectric constant to 28-30, and the linewidth is lower, so that the ferrite material belongs to a basic material which can meet the requirements of reducing the size and improving the performance of microwave devices.
However, as the size of the device is further reduced, the dielectric constant needs to be further improved, so that the NiCuZn spinel ferrite is adopted according to the application requirements of the microwave device, and the dielectric constant is regulated and controlled by utilizing the characteristics of high saturation magnetization, low cost, stable process and the like, so that the ferrite material with high dielectric constant and stable ferromagnetic resonance line width is obtained, and is beneficial to miniaturization and high performance of the microwave device.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of a coated high-dielectric low-loss microwave ferrite material.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the coated high-dielectric low-loss microwave ferrite material comprises the following steps:
step 1, nickel oxide (NiO), copper oxide (CuO), zinc oxide (ZnO) and iridium dioxide (IrO) 2 ) And ferric oxide (Fe) 2 O 3 ) As raw material according to Ni 0.28 Cu 0.16 Zn 0.56 Fe 2-x Ir x O 4 Raw materials are weighed according to the stoichiometric ratio of (1), wherein x=0.0-0.3;
step 2, preparing the raw materials weighed in the step 1 into a NiCuZn ferrite material according to a process of a solid phase sintering method;
2.1, placing the raw materials weighed in the step 1 into a polytetrafluoroethylene or nylon ball milling tank, and performing ball milling for one time by taking zirconium oxide and deionized water as milling media, wherein the ball milling time is 10-16 hours, and the rotating speed is 200-280 revolutions per minute; taking out after ball milling, drying in a blast drying oven, and presintering for 1-6 hours at 850-1000 ℃ in a high temperature furnace;
2.2, performing secondary ball milling on the presintered material obtained in the step 2.1, wherein zirconia and deionized water are used as milling media, the secondary ball milling time is 8-16 hours, and the rotating speed is 200-280 r/min; taking out after the secondary ball milling is finished, and drying in a blast drying oven at 60-120 ℃;
2.3 granulating the dried powder obtained in the step 2.2, then sintering for 1-8 hours at the temperature of 1000-1200 ℃ to obtain NiCuZn ferrite material, grinding and sieving with a 120-mesh sample sieve for later use;
step 3, deionized water according to the mass ratio: glucose=8: 2, weighing glucose, dissolving in deionized water, stirring and mixing uniformly to prepare a glucose solution;
step 4, adding the NiCuZn ferrite material obtained in the step 2 with the mass equal to that of glucose into the glucose solution obtained in the step 3, transferring the obtained mixed solution into a polytetrafluoroethylene reaction kettle, and putting the reaction kettle into a steel sealing tank for sealing;
step 5, placing the sealed tank in the step 4 into a constant temperature sintering furnace or a constant temperature drying oven, preserving heat for 2-10 hours at 160-200 ℃, and performing hydrothermal reaction to prepare carbon spheres;
and step 6, after the reaction is finished, naturally cooling to room temperature (preventing air pressure in the tank), opening the reaction kettle, and cleaning by filtering, ethanol and deionized water to obtain the high-dielectric low-loss microwave ferrite material.
The invention also provides application of the high-dielectric low-loss microwave ferrite material as a substrate material of a microwave device (a circulator, an isolator, a phase shifter and the like).
The coated high-dielectric low-loss microwave ferrite material provided by the invention has the advantages that the inner core NiCuZn ferrite is based on the NiCuZn ferrite material, the Ir element is adopted for performance regulation, the microwave loss of the material is reduced, and the excellent low-loss ferrite is obtained; the shell is a carbon sphere prepared by a hydrothermal method, has a higher dielectric constant, is coated outside ferrite, and has good uniformity, so that the dielectric constant of the material is improved. The coated high-dielectric low-loss microwave ferrite material prepared by the invention has high dielectric constant (epsilon' =30-60) and low microwave loss (ferromagnetic resonance line width delta H=120-180 Oe) in a microwave frequency band (9.56 GHz), and meets the application requirements of circulators, isolators and phase shifters in the microwave frequency band.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to a coated high-dielectric low-loss microwave ferrite material which adopts a coated structure, wherein the shell is a carbon sphere, and the inner core is Ni 0.28 Cu 0.16 Zn 0.56 Fe 2-x Ir x O 4 The spinel ferrite improves the dielectric constant of the material, maintains the stable ferromagnetic resonance line width of the material and meets the application requirement of microwave devices through the formation of a cladding structure.
2. The coated high-dielectric low-loss microwave ferrite material has high dielectric constant (epsilon' =30-60) and low microwave loss (ferromagnetic resonance line width delta H=120-180 Oe) in a microwave frequency band (9.56 GHz), and meets the application requirements of circulators, isolators and phase shifters in the microwave frequency band.
3. When the coated high-dielectric low-loss microwave ferrite material is used as a substrate of a microwave device, the miniaturization of the microwave device can be well realized, the transmission efficiency of a circulator is improved, the miniaturization and high performance of the microwave device are realized, and a novel material is provided for the application of high-frequency and integrated small-size microwave equipment.
Drawings
FIG. 1 is a flow chart of a method for preparing a coated high dielectric low loss microwave ferrite material according to the present invention.
FIG. 2 is a graph showing the microscopic morphology of NiCuZn ferrite prepared in example 1 of the present invention.
Fig. 3 is a microstructure and schematic diagram of the coated high dielectric low loss microwave ferrite material prepared in example 1 of the present invention.
Fig. 4 shows XRD patterns of the coated high dielectric low loss microwave ferrite materials prepared in examples 1, 2 and 3 of the present invention.
Detailed Description
The technical scheme of the invention is described in detail below with reference to the accompanying drawings and examples.
Example 1
The preparation method of the coated high-dielectric low-loss microwave ferrite material comprises the following steps:
step 1. Nickel (NiO) oxide, copper (CuO) oxide, zinc (ZnO) oxide and ferric oxide (Fe) 2 O 3 ) As raw material according to Ni 0.28 Cu 0.16 Zn 0.56 Fe 2-x Ir x O 4 Stoichiometric ratio of (x=0.0) 2.09g of NiO raw material, 1.27g of CuO raw material, 4.56g of ZnO raw material and Fe were weighed out 2 O 3 15.97g of raw material;
step 2, preparing the raw materials weighed in the step 1 into a NiCuZn ferrite material according to a process of a solid phase sintering method;
2.1, placing the raw materials weighed in the step 1 into a polytetrafluoroethylene ball milling tank, performing one-time ball milling by taking zirconium oxide and deionized water as milling media, wherein the ball milling time is 12 hours, and the rotating speed is 250 revolutions per minute; taking out after ball milling, drying in a blast drying oven, and presintering for 4 hours at 950 ℃ in a high-temperature furnace;
2.2, performing secondary ball milling on the presintered material obtained in the step 2.1, wherein zirconia and deionized water are used as milling media, the secondary ball milling time is 12 hours, and the rotating speed is 250 revolutions per minute; taking out after the secondary ball milling is finished, and drying in a blast drying oven at 80 ℃;
2.3 granulating the dried powder obtained in the step 2.2, then heating to 1100 ℃ at a heating rate of 2 ℃/min, sintering for 4 hours at 1100 ℃ to obtain a NiCuZn ferrite material, grinding and sieving with a 120-mesh sample sieve for later use;
step 3, deionized water according to the mass ratio: glucose=8: 2, weighing 10g of glucose, dissolving in 40mL of deionized water, stirring and mixing uniformly to prepare a glucose solution;
step 4, adding 10g of the NiCuZn ferrite material obtained in the step 2 into the glucose solution obtained in the step 3, transferring the obtained mixed solution into a polytetrafluoroethylene reaction kettle, and putting the reaction kettle into a steel sealing tank for sealing;
step 5, placing the sealed tank in the step 4 into a constant temperature sintering furnace or a constant temperature drying oven, preserving the heat at 190 ℃ for 8 hours, and performing hydrothermal reaction to prepare carbon spheres;
and step 6, after the reaction is finished, naturally cooling to room temperature (pressure in the tank is prevented), opening the reaction kettle, and cleaning by filtering, ethanol and deionized water to obtain the high-dielectric low-loss microwave ferrite material.
Example 2
This embodiment differs from embodiment 1 in that:
the process of step 1 is adjusted as follows: with nickel oxide (NiO), copper oxide (CuO), zinc oxide (ZnO), iridium dioxide (IrO) 2 ) And ferric oxide (Fe) 2 O 3 ) As raw material according to Ni 0.28 Cu 0.16 Zn 0.56 Fe 2-x Ir x O 4 Stoichiometric ratio of (x=0.15) NiO raw material 2.09g, cuO raw material 1.27g, znO raw material 4.56g, irO were weighed out 2 3.36g of raw material Fe 2 O 3 14.77g of raw material; the remaining steps were the same as in example 1.
Example 3
This embodiment differs from embodiment 1 in that:
the process of step 1 is adjusted as follows: with nickel oxide (NiO), copper oxide (CuO), zinc oxide (ZnO), iridium dioxide (IrO) 2 ) And ferric oxide (Fe) 2 O 3 ) As raw material according to Ni 0.28 Cu 0.16 Zn 0.56 Fe 2-x Ir x O 4 Stoichiometric ratio of (x=0.3) NiO raw material 2.09g, cuO raw material 1.27g, znO raw material 4.56g, irO were weighed out 2 Raw material 6.73g, fe 2 O 3 13.57g of raw material; the remaining steps were the same as in example 1.
Fig. 2 is a microscopic morphology diagram of the NiCuZn ferrite prepared in example 1 of the present invention, and it can be seen from the figure that the NiCuZn ferrite material has smaller crystal grains and good uniformity and dispersibility.
Fig. 3 is a microstructure diagram and a schematic diagram of a coated high dielectric low loss microwave ferrite material prepared in embodiment 1 of the present invention, and it can be seen from the diagram that the carbon sphere is formed better, some small particles are NiCuZn ferrite on the surface, niCuZn particles are contained in the interior, and the schematic diagram also shows that the NiCuZn material has a small size and enters the interior of the carbon sphere.
Fig. 4 shows XRD patterns of the coated high dielectric low loss microwave ferrite materials prepared in examples 1, 2 and 3 according to the present invention, and it can be seen from the figures that the materials have carbon phase and NiCuZn spinel phase, which are illustrated as two phases coexisting.
The results of the ferromagnetic resonance linewidths and dielectric constants of the materials obtained in example 1, example 2 and example 3 are shown in table 1. The material has a lower ferromagnetic resonance line width and a higher dielectric constant at the microwave frequency of 9.5 GHz. According to the result, the coated high-dielectric low-loss microwave ferrite material prepared by the embodiment has high dielectric constant and low ferromagnetic resonance linewidth coefficient, and can be used as a substrate material of a microwave device.
TABLE 1
Claims (2)
1. The preparation method of the coated high-dielectric low-loss microwave ferrite material is characterized by comprising the following steps of:
step 1, niO, cuO, znO, irO 2 And Fe (Fe) 2 O 3 As raw material according to Ni 0.28 Cu 0.16 Zn 0.56 Fe 2-x Ir x O 4 Raw materials are weighed according to the stoichiometric ratio of (1), wherein x=0.0-0.3;
step 2, preparing the raw materials weighed in the step 1 into a NiCuZn ferrite material according to a process of a solid phase sintering method;
2.1, ball milling the raw materials weighed in the step 1 for one time, wherein the ball milling time is 10-16 hours, and the rotating speed is 200-280 r/min; taking out after ball milling, drying, and presintering for 1-6 hours at 850-1000 ℃;
2.2, performing secondary ball milling on the presintered material obtained in the step 2.1, wherein the secondary ball milling time is 8-16 hours, and the rotating speed is 200-280 r/min; taking out and drying after the secondary ball milling is completed;
2.3 granulating the dried powder obtained in the step 2.2, and then sintering for 1-8 hours at the temperature of 1000-1200 ℃ to obtain the NiCuZn ferrite material;
step 3, deionized water according to the mass ratio: glucose=8: 2, weighing glucose, dissolving in deionized water, stirring and mixing uniformly to prepare a glucose solution;
step 4, adding the NiCuZn ferrite material obtained in the step 2 with the mass equal to that of glucose into the glucose solution obtained in the step 3, transferring the obtained mixed solution into a reaction kettle, and putting the reaction kettle into a steel sealing tank for sealing;
step 5, placing the sealed tank in the step 4 into a constant temperature sintering furnace or a constant temperature drying oven, and preserving heat for 2-10 hours at 160-200 ℃;
and step 6, after the reaction is finished, naturally cooling to room temperature, opening the reaction kettle, and filtering and cleaning to obtain the high-dielectric low-loss microwave ferrite material.
2. Use of the high dielectric low loss microwave ferrite material of claim 1 as a substrate material for microwave devices.
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