CN113461414A - Ferrite suitable for millimeter wave microstrip circulator and preparation method and application thereof - Google Patents
Ferrite suitable for millimeter wave microstrip circulator and preparation method and application thereof Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- 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
- C04B35/2666—Other ferrites containing nickel, copper or cobalt
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/32—Non-reciprocal transmission devices
- H01P1/38—Circulators
- H01P1/383—Junction circulators, e.g. Y-circulators
- H01P1/387—Strip line circulators
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- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6025—Tape casting, e.g. with a doctor blade
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Abstract
The invention belongs to the technical field of microwave circulators, and particularly relates to ferrite suitable for a millimeter wave microstrip circulator and a preparation method and application thereof, wherein the ferrite is applied to a K wave band, and the ferrite is NiZn spinel type ferrite prepared by adopting a tape casting process and comprises the following raw materials in percentage by mole: 49-51 mol% of Fe2O3, 17-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO; the preparation method of the ferrite comprises the processes of ball milling, presintering, tape casting and sintering the ferrite raw material for multiple times; the micro-strip circulator/micro-strip isolator prepared from the ferrite can be suitable for a K wave band and has the advantages of small insertion loss and high performance of the micro-strip circulator/micro-strip isolator.
Description
Technical Field
The invention belongs to the technical field of microwave circulators, and particularly relates to ferrite suitable for a millimeter wave microstrip circulator and a preparation method and application thereof.
Background
Microwave/millimeter wave ferrite circulators, isolators, phase shifters, variable polarizers and other devices play an important role in the microwave technology field, and are widely applied to the fields of aerospace, satellite communication, electronic countermeasure, mobile communication, medical treatment and the like. In circuits and systems such as a receiving/transmitting (T/R) component of a microwave radio frequency front end, a ferrite circulator/isolator and the like play an important role. For the system, raising the frequency is a direct means for improving the data transmission efficiency, and this is also the main reason why the operating spectrum of 5G mobile communication is shifted to the millimeter wave band. Except in the military field such as radar, the mobile communication base station is the largest application of the circulator/isolator. With the rapid development of microwave technology, the requirement of a system on the miniaturization of components is more and more urgent, and the volume of ferrite components is far higher than that of other components, so the tasks of miniaturization, light weight and planarization are particularly urgent. In particular, the miniaturization and the planarization of the millimeter wave circulator and the isolator.
The microstrip circulator can just meet the requirements, plays a role in impedance matching and decoupling in an integrated circuit, and has the characteristics of small volume, light weight, good performance, convenience in realizing monolithic hybrid integration and the like. The micro-strip circulator is a new achievement for developing the application of the micro-strip circulator to higher frequency while meeting the requirements of customers, and the development of the micro-strip circulator has positive significance for the integration of the complete machine, the weight reduction of the complete machine, and the improvement and the stabilization of the comprehensive capacity of the complete machine.
The ferrite is a core material of the circulator/isolator, and the ferrite has the characteristics of high-power bearing operation capacity, low loss, high stability and reliability and the like. In fact, the existing ferrite used for the K wave band has low performance and large loss. The Ni-based spinel ferrite material has the advantages of high saturation magnetization, high Curie temperature and the like, but a porous structure is easy to appear in the sintering process, and the density is low, so the resonance linewidth delta H is large, and the insertion loss of a manufactured microstrip device is large.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problems to be solved by the invention are as follows: the problem that the insertion loss of a manufactured microstrip circulator is large due to the fact that the resonance line width of the Ni-series spinel ferrite is large is solved.
In order to solve the technical problems, the invention adopts the technical scheme that:
the ferrite suitable for the millimeter wave microstrip circulator is provided, the ferrite is applied to a K wave band, and the ferrite is NiZn spinel type ferrite prepared by adopting a tape casting process and comprises the following raw materials in percentage by mole:
49～51mol％Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO.
The composite material comprises the following raw materials in percentage by mole:
49mol％Fe2O319 mol% ZnO, 4 mol% CuO, 0.3 mol% CoO, and 27.7 mol% NiO. Further provides a preparation method of the ferrite suitable for the millimeter wave microstrip circulator, which comprises the following steps:
s1, mixing the following raw materials in percentage by mol:
49～51mol％Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO to obtain a mixed raw material;
s2, performing primary ball milling on the mixed raw materials;
s3, pre-burning the ball-milled mixed raw materials in air to obtain a pre-burned material;
s4, performing secondary ball milling on the pre-sintered material, and sieving the pre-sintered material through a standard sample separation sieve to obtain pre-sintered material powder;
s5, adding 50 wt% of organic binder and 50 wt% of absolute ethyl alcohol into the pre-sintered powder, and continuing ball milling to obtain slurry;
s6, carrying out tape casting on the slurry, and carrying out tape casting at 40 ℃ to obtain a raw film tape with the thickness of 40-60 mu m;
s7, laminating 8-10 layers of green film tapes, and pressing under 6-8MPa to form green sheets of 40-60 mu m;
s8, sintering the green sheet in air at 950-1050 ℃ to obtain the ferrite.
Wherein, zirconium balls are adopted as the grinding balls for ball milling in S2, S4 and S5.
Wherein the pre-sintering temperature is 800 ℃, and the pre-sintering time is 2 h.
Wherein the mesh number of the standard sample separating sieve is 40-60.
Wherein in S6, the blade height of the casting is 600 μm, and the speed of the casting is 120 cm/min.
Wherein the organic binder is PVA.
Further provides the application of the ferrite suitable for the millimeter wave microstrip circulator or the ferrite obtained by the ferrite preparation method on the microstrip circulator/microstrip isolator.
The invention has the beneficial effects that: on the basis of main components of iron oxide, zinc oxide and nickel oxide, a small amount of cobalt oxide and copper oxide are added, and a flow casting process is used for preparing NiZn spinel type ferrite suitable for K wave bands, so that the problem that the Ni spinel type ferrite has larger resonance line width due to the porous structure, low density and the like of the sintered Ni spinel type ferrite can be effectively solved, and the insertion loss of a microstrip circulator prepared from the Ni spinel type ferrite can be reduced; compared with the traditional sintered bulk material, the ferrite prepared by the tape casting process can effectively reduce the production cost of the ferrite and improve the performance of the ferrite.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The invention provides ferrite suitable for a millimeter wave microstrip circulator, which is applied to a K wave band, is NiZn spinel type ferrite prepared by adopting a tape casting process and comprises the following raw materials in percentage by mole:
49～51mol％Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO.
Preferably, the ferrite comprises the following raw materials in percentage by mole:
49mol％Fe2O3，19mol％ZnO，4mol％CuO，0.3mol％CoO，27.7mol％NiO。
specifically, the ferrite 4 pi Ms obtained by the invention is 4200Gs-4500Gs, and the dielectric constant epsilonr13-13.5, Curie temperature of more than or equal to 350--4-2.53×10-4And the ferromagnetic resonance line width delta H is less than or equal to 80 oe.
The preparation method of the ferrite suitable for the millimeter wave microstrip circulator comprises the following steps:
s1, mixing the following raw materials in percentage by mol:
49～51mol％Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO to obtain a mixed raw material;
s2, performing primary ball milling on the mixed raw materials;
s3, pre-burning the ball-milled mixed raw materials in air to obtain a pre-burned material;
s4, performing secondary ball milling on the pre-sintered material, and sieving the pre-sintered material through a standard sample separation sieve to obtain pre-sintered material powder;
s5, adding 50 wt% of organic binder and 50 wt% of absolute ethyl alcohol into the pre-sintered powder, and continuing ball milling to obtain slurry;
s6, carrying out tape casting on the slurry, and carrying out tape casting at 40 ℃ to obtain a raw film tape with the thickness of 40-60 mu m;
s7, laminating 8-10 layers of green film tapes, and pressing under 6-8MPa to form green sheets of 40-60 mu m;
s8, sintering the green sheet in air at 950-1050 ℃ to obtain the ferrite.
Further, zirconium balls were used as the milling balls for the ball milling in S2, S4 and S5.
Further, the pre-sintering temperature is 800 ℃, and the pre-sintering time is 2 hours.
Furthermore, the mesh number of the standard sample separating sieve is 40-60.
Further, in S6, the blade height of the casting was 600 μm, and the speed of the casting was 120 cm/min.
Further, the organic binder is PVA.
Preferably, the preparation method of the ferrite suitable for the millimeter wave microstrip circulator comprises the following steps:
s1, mixing the following raw materials in percentage by mol, and mixing 49-51 mol% of Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30 mol% of NiO to obtain a mixed raw material;
s2, performing first ball milling on the mixed raw materials, wherein the weight ratio of the mixed raw materials to zirconium balls in the first ball milling is 1:4.5, and the first ball milling time is 4 hours;
and S3, pre-burning the ball-milled mixed raw materials in air at 800 ℃ for 2h to obtain a pre-burned material.
S4, performing secondary ball milling on the pre-sintered material by using zirconium balls, wherein the ball milling time is 6 hours, the weight ratio of the pre-sintered material to the zirconium balls is 1:5, and sieving the ball-milled pre-sintered material by using a 40-60-mesh target standard sample sieve to obtain pre-sintered material powder;
s5, adding 50 wt% of PVA and 50 wt% of absolute ethyl alcohol into the pre-sintered powder to obtain mixed slurry;
s6, continuing ball milling the mixed slurry for 6 hours by using zirconium balls to obtain slurry;
s7, casting the slurry on a polypropylene film by adopting a precision casting device, wherein the height of a scraper is 600 mu m, the casting speed is 120cm/min, and a raw film belt with the thickness of 40-60 mu m is obtained by casting at 40 ℃;
s8, laminating 8-10 layers of green film tapes, and pressing under 6-8MPa to form green sheets of 40-60 mu m;
s9, sintering the green sheet in air at 950-1050 ℃ for 2h to obtain the ferrite.
Example one
The ferrite suitable for the millimeter wave microstrip circulator comprises the following raw materials in percentage by mole:
49mol％Fe2O3，19mol％ZnO，4mol％CuO，0.3mol％CoO，27.7mol％NiO。
the preparation method of the ferrite suitable for the millimeter wave microstrip circulator comprises the following steps:
s1, mixing the following raw materials according to the mol percentage of 49mol percent of Fe2O319 mol% of ZnO, 4 mol% of CuO, 0.3 mol% of CoO and 27.7 mol% of NiO to obtain a mixed raw material;
s2, performing first ball milling on the mixed raw materials, wherein the weight ratio of the mixed raw materials to zirconium balls in the first ball milling is 1:4.5, and the first ball milling time is 4 hours;
and S3, pre-burning the ball-milled mixed raw materials in air at 800 ℃ for 2h to obtain a pre-burned material.
S4, performing secondary ball milling on the pre-sintered material by using zirconium balls, wherein the ball milling time is 6 hours, the weight ratio of the pre-sintered material to the zirconium balls is 1:5, and sieving the ball-milled pre-sintered material by using a 60-target standard sample sieve to obtain pre-sintered material powder;
s5, adding 50 wt% of PVA and 50 wt% of absolute ethyl alcohol into the pre-sintered powder to obtain mixed slurry;
s6, continuing ball milling the mixed slurry for 6 hours by using zirconium balls to obtain slurry;
s7, casting the slurry on a polypropylene film by adopting a precision casting device, wherein the height of a scraper is 600 mu m, the casting speed is 120cm/min, and a raw film belt with the thickness of 50 mu m is obtained by casting at 40 ℃;
s8, laminating the 8 layers of green film tapes, and pressing into a green sheet with the thickness of 40 mu m under the pressure of 6 MPa;
s9, sintering the green sheet in the air at 1000 ℃ for 2h to obtain the ferrite.
Detection example 1
The ferrite obtained in the first example was subjected to performance tests, and the results of the performance tests are shown in table 1:
TABLE 1
| Performance of | 4πMs(Gs) | Tc(℃) | △H(oe) | εr | Tanδ |
| Ferrite | 4450 | 382 | 77 | 13.5 | 2.85×10-4 |
Example two
The performance test of the microstrip isolator is performed under the test condition of the K wave band, the microstrip isolator is prepared by the ferrite obtained in the first embodiment, and the performance test result is shown in the table 2:
TABLE 2
In summary, the ferrite suitable for the millimeter wave microstrip circulator provided by the invention is prepared by adding a small amount of cobalt oxide and copper oxide on the basis of main components of iron oxide, zinc oxide and nickel oxide and preparing NiZn spinel ferrite suitable for K wave band through a tape casting process, so that the problem of larger resonance line width of Ni spinel ferrite due to the porous structure and low density of the sintered Ni spinel ferrite is effectively solved, and the insertion loss of the microstrip circulator prepared from the Ni spinel ferrite is reduced; compared with the traditional sintered bulk material, the ferrite prepared by the tape casting process can effectively reduce the production cost of the ferrite and improve the performance of the ferrite.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (9)
1. The ferrite suitable for the millimeter wave microstrip circulator is characterized in that the ferrite is applied to a K wave band, is NiZn spinel type ferrite prepared by adopting a tape casting process and comprises the following raw materials in percentage by mole:
49～51mol％Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO.
2. The ferrite suitable for the millimeter wave microstrip circulator of claim 1, comprising the following raw materials by mole percent:
49mol％Fe2O3，19mol％ZnO，4mol％CuO，0.3mol％CoO，27.7mol％NiO。
3. the preparation method of the ferrite suitable for the millimeter wave microstrip circulator is characterized by comprising the following steps of:
s1, mixing the following raw materials in percentage by mol:
49～51mol％Fe2O317-19 mol% of ZnO, 3-4 mol% of CuO, 0.2-0.5 mol% of CoO and 25-30% of NiO to obtain a mixed raw material;
s2, performing primary ball milling on the mixed raw materials;
s3, pre-burning the ball-milled mixed raw materials in air to obtain a pre-burned material;
s4, performing secondary ball milling on the pre-sintered material, and sieving the pre-sintered material through a standard sample separation sieve to obtain pre-sintered material powder;
s5, adding 50 wt% of organic binder and 50 wt% of absolute ethyl alcohol into the pre-sintered powder, and continuing ball milling to obtain slurry;
s6, carrying out tape casting on the slurry, and carrying out tape casting at 40 ℃ to obtain a raw film tape with the thickness of 40-60 mu m;
s7, laminating 8-10 layers of green film tapes, and pressing under 6-8MPa to form green sheets of 40-60 mu m;
s8, sintering the green sheet in air at 950-1050 ℃ to obtain the ferrite.
4. The method for preparing ferrite suitable for millimeter wave microstrip circulator of claim 3 wherein zirconium balls are used as milling balls in S2, S4 and S5.
5. The method for preparing the ferrite suitable for the millimeter wave microstrip circulator as claimed in claim 3, wherein the pre-sintering temperature is 800 ℃ and the pre-sintering time is 2 h.
6. The preparation method of the ferrite suitable for the millimeter wave microstrip circulator as claimed in claim 3, wherein the mesh number of the standard sample separation sieve is 40-60.
7. The method of claim 3, wherein in S6, the blade height of the casting is 600 μm, and the casting speed is 120 cm/min.
8. The method of claim 3, wherein the organic binder is PVA.
9. Use of the ferrite suitable for millimeter wave microstrip circulator of any one of claims 1 to 7 in the preparation of microstrip circulator/microstrip isolator.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115925404A (en) * | 2022-10-24 | 2023-04-07 | 深圳市华扬通信技术有限公司 | YIG ferrite substrate, preparation method thereof and microstrip circulator/isolator |
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| US3344072A (en) * | 1963-02-28 | 1967-09-26 | Nippon Electric Co | Tantalum doped nickel-zinc ferrite |
| US6436307B1 (en) * | 1999-06-29 | 2002-08-20 | Thomson-Csf | Low loss ferrites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115925404A (en) * | 2022-10-24 | 2023-04-07 | 深圳市华扬通信技术有限公司 | YIG ferrite substrate, preparation method thereof and microstrip circulator/isolator |
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Application publication date: 20211001 |