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CN112047731A - Hexagonal ferrite material for quasi-planar microstrip circulator and preparation method thereof - Google Patents

Hexagonal ferrite material for quasi-planar microstrip circulator and preparation method thereof Download PDF

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CN112047731A
CN112047731A CN202010880100.3A CN202010880100A CN112047731A CN 112047731 A CN112047731 A CN 112047731A CN 202010880100 A CN202010880100 A CN 202010880100A CN 112047731 A CN112047731 A CN 112047731A
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parts
temperature
preparation
quasi
weight
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CN112047731B (en
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李之琦
罗会安
王文鑫
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Nanjing Glarun Microwave Devices Co ltd
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Nanjing Glarun Microwave Devices Co ltd
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Abstract

The invention discloses a hexagonal ferrite material for a quasi-planar microstrip circulator, which comprises main materials and additives, wherein the main materials comprise the following components in parts by weight: fe2O3 40 to 90 parts of BaCO3 5 to 10 parts of La2O3 1 to 10 parts of Sc2O3 2-5 parts; the additive comprises the following components in percentage by weight: 1 to 10 parts of CuO and Bi2O3 1-10 parts. The invention also discloses a preparation method of the hexagonal ferrite. The hexaferrite material for the quasi-planar microstrip circulator prepared by the method has excellent performances of higher coercive force, low ferromagnetic resonance line width, high Curie temperature and the like.

Description

Hexagonal ferrite material for quasi-planar microstrip circulator and preparation method thereof
Technical Field
The invention belongs to the technical field of electronic materials, and particularly relates to a hexagonal ferrite material for a quasi-planar microstrip circulator and a preparation method thereof.
Background
With the continuous development of semiconductor technology and the urgent requirements of a complete machine system on high frequency, miniaturization, light weight and high reliability of microwave devices, the application problem of microstrip circulators in radar systems such as satellite-borne radars, air defense systems, precise guidance, gun aiming measurement, remote early warning and the like is increasingly prominent. The main bottleneck for restricting the microstrip circulator to achieve the goals of miniaturization, light weight, planarization and high reliability is the self-bias hexaferrite material with the characteristics of low delta H, high Mr/Ms and high Ha applied to the microstrip circulator.
The hexagonal ferrite material has high coercive force, high remanence ratio and strong anisotropy. The high coercive force can keep the permanent magnetic property of the hexagonal ferrite material, the high remanence ratio can make the magnetic moment tend to the direction precession of strong anisotropy, and the high anisotropy can generate a large 'internal field' in the ferrite, so that the magnetic moment generates ferromagnetic resonance with the microwave/millimeter wave under the condition of no external steady magnetic field or small steady magnetic field. The advantage of the hexagonal ferrite material can provide a self-bias field for the operation of the micro-strip circulator, completely get rid of the permanent magnet with the thickness of about 2mm, and achieve the purposes of miniaturization, light weight and high reliability.
The performance of the prior hexagonal ferrite material still has the problems of high ferromagnetic resonance line width, low remanence ratio, low temperature stability and the like.
Based on abundant practical experience and professional knowledge for many years of design and manufacture of the product, the inventor of the invention actively carries out research and innovation by matching with the application of theories so as to create the hexaferrite material for the quasi-planar microstrip circulator and the preparation method thereof, and can effectively improve the prior art. The inventor of the invention finally creates the invention with practical value after continuous research and design and repeated trial and improvement.
Disclosure of Invention
The invention mainly aims to overcome the defects in the prior art and provides a hexaferrite material for a quasi-planar microstrip circulator and a preparation method thereof. The hexagonal ferrite material for the quasi-planar microstrip circulator has excellent performances of high coercive force, low ferromagnetic resonance line width, high remanence ratio, high Curie temperature and the like.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides a hexagonal ferrite material for a quasi-planar microstrip circulator, which comprises main materials and additives, wherein the main materials comprise the following components in parts by weight: fe2O3 40 to 90 parts of BaCO3 5 to 10 parts of La2O3 1 to 10 parts of Sc2O3 2-5 parts; the additive comprises the following components in percentage by weight: 1 to 10 parts of CuO and Bi2O3 1-10 parts.
The purpose of the invention and the technical problem to be solved are also realized by adopting the following technical scheme.
The invention provides a hexagonal ferrite material for a quasi-planar microstrip circulator, which comprises main materials and additives, wherein the main materials comprise the following components in parts by weight: fe2O3 40 to 90 parts of BaCO3 5 to 10 parts of La2O3 1 to 10 parts of Sc2O3 2-5 parts; the additive comprises the following components in percentage by weight: 1 to 10 parts of CuO and Bi2O3 1 to 10 parts of SiO2 0.01 to 0.5 part of CaCO3 0.01-4 parts.
Further, the main material comprises the following components in parts by weight: fe2O3 50-90 parts of BaCO3 6-10 parts of La2O3 6 to 10 parts of Sc2O3 3-5 parts; the additive comprises the following components in percentage by weight: 1 to 4.5 parts of CuO and Bi2O3 1 to 4.5 parts of SiO2 0.01 to 0.5 part of CaCO3 0.01-4 parts.
The purpose of the invention and the technical problem to be solved are also realized by adopting the following technical scheme.
The invention provides a method for preparing a hexagonal ferrite material for a quasi-planar microstrip circulator, which comprises the following steps of:
1) primary ball milling: weighing the main materials according to the proportion, putting the main materials into a ball mill, adding a dispersing agent, grinding, crushing and uniformly mixing;
2) and (3) calcining: drying the obtained ball milling material, and calcining in a furnace;
3) secondary ball milling: putting the calcined components into a ball mill, adding an additive and a dispersant, grinding and crushing for the second time, and mixing uniformly;
4) and (3) dehydrating: dehydrating the slurry subjected to secondary grinding and crushing;
5) molding: pressing the obtained dehydrated slurry into a blank in a magnetic field environment by a wet method, wherein the magnetic field intensity is more than 1.5T;
6) and (3) sintering: and putting the obtained blank into a furnace for sintering.
Further, the ball milling conditions in the step 1) are as follows: the rotation speed is 50-80 r/min, and the grinding time is 5-25 h.
Further, the drying conditions in the step 2) are as follows: the temperature is 90-130 ℃, and the time is 20-30 h.
Further, the calcining mode in the step 2) is a program calcining mode, the temperature rising speed is 50 ℃/h within 0-5 h, the temperature rising speed is 90 ℃/h within 5-12 h, the temperature is kept for 4h when the temperature rises to 800-1300 ℃, and the temperature is reduced to the room temperature at the speed of 15-20 ℃/h after the temperature is kept.
Further, the ball milling conditions in the step 3) are as follows: the rotation speed is 50-80 r/min, and the grinding time is 16-25 h.
Further, after the dehydration treatment in the step 4), the water content of the dehydrated slurry is controlled to be 15-25%.
Further, the calcining mode in the step 6) is a program calcining mode, the temperature rising speed is 25-40 ℃/h within 0-10 h, the temperature is kept for 4h when the temperature rises to 700-1200 ℃, the temperature is reduced at the speed of 50 ℃/h after the temperature is kept, and then the temperature is reduced to the room temperature along with furnace air cooling.
By the technical scheme, the invention at least has the following advantages: the hexaferrite material for the quasi-planar microstrip circulator prepared by the method has excellent performances of higher coercive force, low ferromagnetic resonance line width, high Curie temperature and the like.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Weighing 829g Fe2O3、89g BaCO3、73g La2O3、32g Sc2O3Respectively putting the mixture into a ball mill, adding deionized water, grinding and crushing, wherein the ball milling time is 8 hours, and the rotating speed of the ball mill is 70 r/min; uniformly mixing the ground and crushed components, and then putting the mixture into a 120 ℃ oven to dry for 24 hours; putting the dried components into a furnace for calcination, wherein the calcination mode is a program calcination mode, the temperature rise speed is 50 ℃/h within 0-4 h, the temperature rise speed is 92 ℃/h within 4-11 h, and the temperature is raised to 1250 ℃ for heat preservation for 4 h; naturally cooling to room temperature along with air in the furnace after heat preservation; the calcined components are put into a ball mill, and 30g of CuO and 25g of Bi as additives are added2O3、6g SiO2、6g CaCO3Grinding and crushing with distilled water, wherein the ball milling time is 18h, and the rotating speed of a ball mill is 70 r/min; dehydrating the ground slurry, and controlling the water content to be about 20%; pressing the obtained dehydrated slurry into a blank in a magnetic field environment with the magnetic field intensity of more than 1.5T by a wet method; sintering the blank in a sintering furnace, wherein the sintering mode is a temperature programming mode, the temperature rising speed is 25-40 ℃/h in 0-10 h,the temperature is increased to 1040 ℃ and kept for 4 h; and (4) cooling at the speed of 50 ℃/h after heat preservation, and then cooling to room temperature along with furnace air cooling to obtain the hexagonal ferrite material.
Example 2
813g of Fe were weighed2O3、89g BaCO3、73g La2O3、32g Sc2O3Respectively putting the mixture into a ball mill, adding deionized water, grinding and crushing, wherein the ball milling time is 8 hours, and the rotating speed of the ball mill is 70 r/min; uniformly mixing the ground and crushed components, and then putting the mixture into a 120 ℃ oven to dry for 24 hours; putting the dried components into a furnace for calcination, wherein the calcination mode is a program calcination mode, the temperature rise speed is 50 ℃/h within 0-4 h, the temperature rise speed is 92 ℃/h within 4-11 h, and the temperature is raised to 1250 ℃ for heat preservation for 4 h; naturally cooling to room temperature along with air in the furnace after heat preservation; the calcined components are put into a ball mill, and 30g of CuO and 25g of Bi as additives are added2O3Grinding and crushing with distilled water, wherein the ball milling time is 18h, and the rotating speed of a ball mill is 70 r/min; dehydrating the ground slurry, and controlling the water content to be about 20%; pressing the obtained dehydrated slurry into a blank in a magnetic field environment with the magnetic field intensity of more than 1.5T by a wet method; sintering the blank in a sintering furnace, wherein the sintering mode is a temperature programming mode, the temperature rising speed is 25-40 ℃/h in 0-10 h, and the temperature rises to 1050 ℃ and is kept for 4 h; and (4) cooling at the speed of 50 ℃/h after heat preservation, and then cooling to room temperature along with furnace air cooling to obtain the hexagonal ferrite material.
Example 3
842g of Fe are weighed2O3、124g BaCO3、44g La2O3、18g Sc2O3Respectively putting the mixture into a ball mill, adding deionized water, grinding and crushing, wherein the ball milling time is 8 hours, and the rotating speed of the ball mill is 70 r/min; uniformly mixing the ground and crushed components, and then putting the mixture into a 120 ℃ oven to dry for 24 hours; putting the dried components into a furnace for calcination, wherein the calcination mode is a program calcination mode, the temperature rise speed is 50 ℃/h in 0-4 h, the temperature rise speed is 92 ℃/h in 4-11 h, and the temperature rises to 125 DEG CKeeping the temperature at 0 ℃ for 4 h; naturally cooling to room temperature along with air in the furnace after heat preservation; the calcined components are put into a ball mill, and 30g of CuO and 25g of Bi as additives are added2O3、6g SiO2、6g CaCO3Grinding and crushing with distilled water, wherein the ball milling time is 18h, and the rotating speed of a ball mill is 70 r/min; dehydrating the ground slurry, and controlling the water content to be about 20%; pressing the obtained dehydrated slurry into a blank in a magnetic field environment with the magnetic field intensity of more than 1.5T by a wet method; sintering the blank in a sintering furnace, wherein the sintering mode is a temperature programming mode, the temperature rising speed is 25-40 ℃/h in 0-10 h, and the temperature rises to 1060 ℃ and is kept for 4 h; and (4) cooling at the speed of 50 ℃/h after heat preservation, and then cooling to room temperature along with furnace air cooling to obtain the hexagonal ferrite material.
Test example 1 Properties of hexagonal ferrite Material
Test subjects: the hexaferrite materials obtained in examples 1 to 3.
The test method comprises the following steps: measuring the density by adopting a drainage method; measuring the saturation magnetization Ms, the residual magnetization Mr, the Curie temperature Tc, the coercive force Hc and the like by using a vibration sample magnetometer; the ferromagnetic resonance linewidth is characterized by a vector network analyzer under a zero field condition through a coplanar waveguide (GCPW); the magnetocrystalline anisotropy field Ha is given by the ktel equation. The acquisition of the parameters is implemented according to GB/T9633-2012 performance test method for gyromagnetic ferrite material applied in microwave frequency. The results are shown in Table 1.
TABLE 1 Performance indices of Hexahexate materials
Figure 393887DEST_PATH_IMAGE001
As can be seen from table 1, the hexaferrite materials obtained in embodiments 1 to 3 of the present invention have excellent properties such as significantly higher coercivity, low ferromagnetic resonance linewidth, and high curie temperature.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The hexagonal ferrite material for the quasi-planar microstrip circulator comprises main materials and additives, wherein the main materials comprise the following components in parts by weight: fe2O3 40 to 90 parts of BaCO3 5 to 10 parts of La2O3 1 to 10 parts of Sc2O3 2-5 parts; the additive comprises the following components in percentage by weight: 1 to 10 parts of CuO and Bi2O3 1-10 parts.
2. The hexagonal ferrite material for the quasi-planar microstrip circulator comprises main materials and additives, wherein the main materials comprise the following components in parts by weight: fe2O3 40 to 90 parts of BaCO3 5 to 10 parts of La2O3 1 to 10 parts of Sc2O3 2-5 parts; the additive comprises the following components in percentage by weight: 1 to 10 parts of CuO and Bi2O3 1 to 10 parts of SiO2 0.01 to 0.5 part of CaCO3 0.01-4 parts.
3. The hexaferrite material for the quasi-planar microstrip circulator of claim 2, wherein the main material comprises the following components in parts by weight: fe2O3 50-90 parts of BaCO3 6-10 parts of La2O3 6 to 10 parts of Sc2O3 3-5 parts; the additive comprises the following components in percentage by weight: 1 to 4.5 parts of CuO and Bi2O3 1 to 4.5 parts of SiO2 0.01 to 0.5 part of CaCO3 0.01-4 parts.
4. A method of preparing a hexaferrite material for a quasi-planar microstrip circulator, the method comprising the steps of:
1) primary ball milling: weighing the main materials according to the proportion, putting the main materials into a ball mill, adding a dispersing agent, grinding, crushing and uniformly mixing;
2) and (3) calcining: drying the obtained ball milling material, and calcining in a furnace;
3) secondary ball milling: putting the calcined components into a ball mill, adding an additive and a dispersant, grinding and crushing for the second time, and mixing uniformly;
4) and (3) dehydrating: dehydrating the slurry subjected to secondary grinding and crushing;
5) molding: pressing the obtained dehydrated slurry into a blank in a magnetic field environment by a wet method, wherein the magnetic field intensity is more than 1.5T;
6) and (3) sintering: and putting the obtained blank into a furnace for sintering.
5. The preparation method according to claim 4, wherein the ball milling conditions in the step 1) are as follows: the rotation speed is 50-80 r/min, and the grinding time is 5-25 h.
6. The preparation method according to claim 4, wherein the drying condition in the step 2) is: the temperature is 90-130 ℃, and the time is 20-30 h.
7. The preparation method of claim 4, wherein the calcination in the step 2) is a procedure calcination, the temperature rising speed is 50 ℃/h within 0-5 h, the temperature rising speed is 90 ℃/h within 5-12 h, the temperature is kept for 4h when the temperature rises to 800-1300 ℃, and the temperature is reduced to room temperature at the speed of 15-20 ℃/h after the temperature is kept.
8. The preparation method according to claim 4, wherein the ball milling conditions in the step 3) are as follows: the rotation speed is 50-80 r/min, and the grinding time is 16-25 h.
9. The preparation method of claim 4, wherein after the dehydration treatment in the step 4), the water content of the dehydrated slurry is controlled to be 15-25%.
10. The preparation method of claim 4, wherein the calcination manner in the step 6) is a procedure calcination manner, the temperature rising speed is 25-40 ℃/h within 0-10 h, the temperature is kept for 4h after the temperature rises to 700-1200 ℃, and then the temperature is reduced at the speed of 50 ℃/h after the temperature is kept, and then the temperature is cooled to the room temperature with furnace air cooling.
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CN112830776A (en) * 2021-03-25 2021-05-25 电子科技大学 A kind of U-shaped hexagonal ferrite material and preparation method thereof
CN112939590A (en) * 2021-03-12 2021-06-11 电子科技大学 Hexahexaferrite material for X-band quasi-planar device and preparation method thereof
CN113078429A (en) * 2021-03-12 2021-07-06 电子科技大学 Quasi-planar composite substrate microstrip circulator
CN113072369A (en) * 2021-03-25 2021-07-06 电子科技大学 U-shaped hexagonal ferrite material with high remanence ratio and preparation method thereof

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CN112939590A (en) * 2021-03-12 2021-06-11 电子科技大学 Hexahexaferrite material for X-band quasi-planar device and preparation method thereof
CN113078429A (en) * 2021-03-12 2021-07-06 电子科技大学 Quasi-planar composite substrate microstrip circulator
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CN113072369A (en) * 2021-03-25 2021-07-06 电子科技大学 U-shaped hexagonal ferrite material with high remanence ratio and preparation method thereof

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