CN110078492B - Magnesium ferrite based low-loss magnetic dielectric material and preparation method thereof - Google Patents

Magnesium ferrite based low-loss magnetic dielectric material and preparation method thereof Download PDF

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CN110078492B
CN110078492B CN201910362184.9A CN201910362184A CN110078492B CN 110078492 B CN110078492 B CN 110078492B CN 201910362184 A CN201910362184 A CN 201910362184A CN 110078492 B CN110078492 B CN 110078492B
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magnesium ferrite
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郭莉
李颉
甘功雯
杨燕
王刚
张怀武
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University of Electronic Science and Technology of China
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Abstract

A magnesium ferrite based low-loss magnetic dielectric material belongs to the field of electronic materials. The magnetic medium material takes magnesium ferrite as a base material,the praseodymium-doped magnesium ferrite material is Mg1‑xCdxFe2‑yPryO4The spinel ferrite material is characterized in that x is 0.1-0.3, and y is 0.02-0.08. The magnetic dielectric material of the invention utilizes the modification of Pr ions to adjust the magnetic property and the dielectric property of the material, realizes that the low-temperature sintering is approximately equal to the magnetic dielectric, simultaneously, the synthesis process of the material controls the crystal grain growth to be uniform, the material has lower magnetic loss parameters, and has equal magnetic dielectric property and low loss factor in the frequency range of 1 MHz-30 MHz; when the magnetic dielectric material is used as an antenna substrate material, the miniaturization of the antenna can be well realized, the radiation efficiency and the bandwidth of the microstrip antenna can be favorably improved, and a new scheme is provided for the design of small-size wireless communication equipment.

Description

Magnesium ferrite based low-loss magnetic dielectric material and preparation method thereof
Technical Field
The invention belongs to the field of electronic materials, and particularly relates to a magnesium ferrite based low-loss magnetic dielectric material and a preparation method thereof.
Background
With the realization of the scale and practicability of 4G communication in the world, the 5G technology has become the key research and development point of the global mobile communication industry. The 5G has huge industrial value and can drive the rapid development of various basic industries such as chips, devices, materials, software and the like. The 5G is more closely integrated with the application of the industries such as the Internet, the Internet of things, industry, traffic, medical treatment and the like, and further a new round of industrial innovation wave is promoted. In the three-network integration construction, various components can not be separated from network equipment or terminal equipment. The reformation and upgrading of the network and the diversified design of the terminal equipment are based on the innovation of key component technology.
Since 5G will use higher frequency, it gradually increases from the past 3GHz down to 6GHz and microwave frequency band, which brings new technical trend for antenna radio frequency material. According to the antenna junctionThe structural size of the antenna is in direct proportion to the wavelength of waves in a medium, and in order to reduce the size, the mass and the volume of the microstrip antenna with a lower frequency band, the structural size is calculated according to the resonant frequency of the antenna
Figure BDA0002047156760000011
It is found that the effective permeability μ of the antenna dielectric substrate is improvedeffThe size of the antenna substrate can be effectively reduced, surface waves are not easy to excite, and radiation of antenna energy is facilitated. Meanwhile, if the effective permeability and the effective permittivity of the substrate material can be made equal, the characteristic impedance of the antenna dielectric substrate
Figure BDA0002047156760000012
That is, the characteristic impedance is equal to that of a vacuum, so that in the miniaturization of the antenna, the antenna substrate material is made of a low-loss magnetic dielectric material, and the negative influence on the antenna gain and the bandwidth caused by the high-dielectric-constant material can be effectively avoided. Meanwhile, the size of the antenna substrate is reduced, and the radiation efficiency of the antenna is improved. Therefore, the isomagnetic materials have been one of the hot spots in the field of antenna. The invention discloses a three-phase composite microstrip antenna substrate material and a preparation method thereof (application number 201410326932.5), which are applied in 2014 by Shouzong et al of Beijing aerospace university, and provides an antenna substrate material compounded by magnetic filler, dielectric filler and a certain amount of polymer. The invention discloses a microstrip antenna organic composite substrate material and a preparation method thereof (application number 20140431104.8), which are applied in 2014 by Subirch et al, a university of electronic technology2The Z barium strontium ferrite material and the polytetrafluoroethylene resin material are compounded to form the equivalent magnetic dielectric material, but a polypropylene resin organic matter adopted in the magnetic dielectric material is greatly influenced by temperature in practical application, and the performance of the antenna is seriously influenced.
Disclosure of Invention
The invention aims to provide a magnesium ferrite based low-loss magnetic dielectric material and a preparation method thereof aiming at the defects in the background art. The magnetic dielectric material of the invention utilizes the modification of Pr ions to adjust the magnetic property and the dielectric property of the material, realizes that the low-temperature sintering is approximately equal to the magnetic dielectric, simultaneously, the synthesis process of the material controls the crystal grain growth to be uniform, the material has lower magnetic loss parameters, and has equal magnetic dielectric property and low loss factor in the frequency range of 1 MHz-30 MHz; when the magnetic dielectric material is used as an antenna substrate material, the miniaturization of the antenna can be well realized, the radiation efficiency and the bandwidth of the microstrip antenna can be favorably improved, and a new scheme is provided for the design of small-size wireless communication equipment.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the magnesium ferrite based low-loss magnetic dielectric material is characterized in that the magnetic dielectric material is obtained by modifying magnesium ferrite serving as a base material by praseodymium doping, and the praseodymium-doped magnesium ferrite material is Mg1-xCdxFe2-yPryO4The spinel ferrite material is characterized in that x is 0.1-0.3, and y is 0.02-0.08; the magnetic dielectric material is prepared by calculating according to the chemical proportion, ball-milling and mixing, drying, sieving, granulating, pressing and molding, and sintering at 900-1200 ℃ for 1-6 hours.
A preparation method of a magnesium ferrite based low-loss magnetic dielectric material comprises the following steps:
step 1: magnesium oxide (MgO), cadmium oxide (CdO) and praseodymium oxide (Pr)2O3) And ferric oxide (Fe)2O3) As raw material, according to the material Mg1-xCdxFe2-yPryO4The ratio of metal elements in the mixture is converted into MgO, CdO and Pr2O3And Fe2O3Weighing, mixing, carrying out primary ball milling, and drying, wherein the value range of x is 0.1-0.3, and the value range of y is 0.02-0.08;
step 2: screening the primary ball-milling dried material obtained in the step 1, putting the screened primary ball-milling dried material into a sintering furnace for presintering, wherein the presintering temperature is 950-1100 ℃ and the time is 2-6 h, and then cooling the presintering material to room temperature along with the furnace to obtain a presintering material;
and step 3: performing secondary ball milling on the pre-sintered material obtained in the step 2 for 12-16 h, controlling the average particle size of powder after the secondary ball milling to be below 2 mu m, and then drying and sieving the secondary ball-milled material;
and 4, step 4: and (3) adding a PVA (polyvinyl alcohol) adhesive into the mixed powder obtained in the step (3), granulating, pressing and forming, sintering at 900-1200 ℃ for 1-6 h, and cooling to room temperature along with the furnace to obtain the magnesium ferrite based low-loss magnetic dielectric material.
Further, the rotation speed of the primary ball milling in the step 1 is 220 rpm, the ball milling time is 16-24 hours, and the ball milling medium is deionized water.
The invention also provides application of the magnesium ferrite based low-loss magnetic dielectric material as a microstrip antenna substrate material.
The invention has the beneficial effects that:
1. the magnesium ferrite based low-loss magnetic dielectric material provided by the invention adopts magnesium ferrite as a main phase material, and Pr is added2O3The performance is regulated, the magnetic performance of the ferrite is reduced, the dielectric constant of the material is regulated, the isomagnetic dielectric material is obtained, the grain growth uniformity of the material is controlled through the process, the loss of the material is reduced, and the material can be used as a substrate material of a microstrip antenna.
2. The magnetic dielectric material realizes low-temperature sintering and approximately equal magnetic dielectric, and has equal magnetic dielectric and low loss factor in the frequency range of 1.0 MHz-30 MHz (the magnetic conductivity and the dielectric constant are both about 12-27, and the specific magnetic loss coefficient and the specific dielectric loss coefficient in a frequency band are both lower than 0.01).
3. When the magnetic dielectric material is used as an antenna substrate material, the miniaturization of the antenna can be well realized, the radiation efficiency and the bandwidth of the microstrip antenna can be favorably improved, and a new scheme is provided for the design of small-size wireless communication equipment.
Drawings
FIG. 1 is a flow chart of a magnesium ferrite-based low-loss magnetic dielectric material and a preparation method thereof;
FIG. 2 is a performance test curve of the magnesium ferrite-based magnetic dielectric material obtained in example 1; wherein, (a) is a performance diagram of magnetic permeability and dielectric constant, and (b) is a performance diagram of magnetic loss and dielectric loss;
FIG. 3 is a performance test curve of the magnesium ferrite-based magnetic dielectric material obtained in example 2; wherein, (a) is a performance diagram of magnetic permeability and dielectric constant, and (b) is a performance diagram of magnetic loss and dielectric loss.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Example 1
A preparation method of a magnesium ferrite-based magnetic dielectric material comprises the following steps:
step 1: magnesium oxide (MgO), cadmium oxide (CdO) and praseodymium oxide (Pr)2O3) And ferric oxide (Fe)2O3) As raw material, according to the material Mg0.8Cd0.2Fe1.96Pr0.04O4The mass of MgO is 3.2g, the mass of CdO is 2.57g, and Pr is calculated according to the ratio of the metal elements in the2O3Has a mass of 0.66g, Fe2O3Weighing the materials, mixing the materials, carrying out primary ball milling for 16 hours, and drying the materials;
step 2: sieving the primary ball-milling dried material obtained in the step 1, putting the sieved material into a sintering furnace for presintering, wherein the presintering temperature is 1000 ℃, the presintering time is 3 hours, and then cooling the presintering material to room temperature along with the furnace to obtain a presintering material;
and step 3: carrying out secondary ball milling on the pre-sintered material obtained in the step 2 for 16h, controlling the average particle size of powder after the secondary ball milling to be below 2 mu m, and then drying and sieving the secondary ball-milled material;
and 4, step 4: and (3) adding a PVA (polyvinyl alcohol) adhesive into the mixed powder obtained in the step (3), granulating, pressing and forming, sintering at 1180 ℃ for 6 hours, and cooling to room temperature along with a furnace to obtain the low-loss magnetic dielectric material based on the magnesium ferrite.
FIG. 2 is a performance test curve of the magnesium ferrite-based magnetic dielectric material obtained in example 1; wherein, (a) is a performance diagram of magnetic permeability and dielectric constant, and (b) is a performance diagram of magnetic loss and dielectric loss; as is clear from FIG. 2, the permeability and the dielectric constant of the magneto-dielectric material obtained in example 1 were maintained at 1MHz to 30MHzAbout 24, while the magnetic loss and the dielectric loss are kept at 10 in the corresponding frequency-2In magnitude.
Example 2
A preparation method of a magnesium ferrite-based magnetic dielectric material comprises the following steps:
step 1: magnesium oxide (MgO), cadmium oxide (CdO) and praseodymium oxide (Pr)2O3) And ferric oxide (Fe)2O3) As raw material, according to the material Mg0.8Cd0.2Fe1.94Pr0.06O4The mass of MgO is 3.2g, the mass of CdO is 2.57g, and Pr is calculated according to the ratio of the metal elements in the2O3Has a mass of 0.99g, Fe2O3Weighing the materials, mixing the materials, carrying out primary ball milling for 16 hours, and drying the materials, wherein the mass of the materials is 15.49 g;
step 2: sieving the primary ball-milling dried material obtained in the step 1, putting the sieved material into a sintering furnace for presintering, wherein the presintering temperature is 1000 ℃, the presintering time is 3 hours, and then cooling the presintering material to room temperature along with the furnace to obtain a presintering material;
and step 3: carrying out secondary ball milling on the pre-sintered material obtained in the step 2 for 16h, controlling the average particle size of powder after the secondary ball milling to be below 2 mu m, and then drying and sieving the secondary ball-milled material;
and 4, step 4: and (3) adding a PVA (polyvinyl alcohol) adhesive into the mixed powder obtained in the step (3), granulating, pressing and forming, sintering at 1180 ℃ for 6 hours, and cooling to room temperature along with a furnace to obtain the low-loss magnetic dielectric material based on the magnesium ferrite.
FIG. 3 is a performance test curve of the magnesium ferrite-based magnetic dielectric material obtained in example 2; wherein, (a) is a performance diagram of magnetic permeability and dielectric constant, and (b) is a performance diagram of magnetic loss and dielectric loss; as is clear from FIG. 3, the magnetocaloric material obtained in example 2 had a permeability and a dielectric constant of about 27, and had a magnetic loss and a dielectric loss of 10-2In magnitude.

Claims (5)

1. The magnesium ferrite based low-loss magnetic dielectric material is characterized in that the magnetic dielectric material is Mg1-xCdxFe2-yPryO4Spinel ferrite material, wherein x is taken fromThe value is 0.1-0.3, and the value of y is 0.02-0.08.
2. The magnesium ferrite based low-loss magnetic dielectric material according to claim 1, wherein the magnetic dielectric material is prepared by taking magnesium oxide, cadmium oxide, praseodymium oxide and ferric oxide as raw materials, weighing the raw materials according to the chemical proportion, mixing by ball milling, drying, sieving, granulating, pressing and molding, and sintering at 900-1200 ℃ for 1-6 hours.
3. A preparation method of a magnesium ferrite based low-loss magnetic dielectric material comprises the following steps:
step 1: with MgO, CdO, Pr2O3And Fe2O3As raw material, according to the material Mg1-xCdxFe2-yPryO4The ratio of metal elements in the mixture is converted into MgO, CdO and Pr2O3And Fe2O3Weighing, mixing, carrying out primary ball milling, and drying, wherein the value range of x is 0.1-0.3, and the value range of y is 0.02-0.08;
step 2: screening the primary ball-milling dried material obtained in the step 1, putting the screened primary ball-milling dried material into a sintering furnace for presintering, wherein the presintering temperature is 950-1100 ℃ and the time is 2-6 h, and then cooling the presintering material to room temperature along with the furnace to obtain a presintering material;
and step 3: performing secondary ball milling on the pre-sintered material obtained in the step 2 for 12-16 h, controlling the average particle size of powder after the secondary ball milling to be below 2 mu m, and then drying and sieving the secondary ball-milled material;
and 4, step 4: and (3) adding a PVA (polyvinyl alcohol) adhesive into the mixed powder obtained in the step (3), granulating, pressing and forming, sintering at 900-1200 ℃ for 1-6 h, and cooling to room temperature along with the furnace to obtain the magnesium ferrite based low-loss magnetic dielectric material.
4. The preparation method of the magnesium ferrite based low-loss magnetic-dielectric material according to claim 3, wherein the rotation speed of the primary ball milling in the step 1 is 220 rpm, the ball milling time is 16-24 hours, and the ball milling medium is deionized water.
5. Use of the magnesium ferrite-based low-loss magnetic dielectric material according to any one of claims 1 to 2 as a microstrip antenna substrate material.
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FR2854981B1 (en) * 2003-05-16 2014-05-23 Thales Sa FERRITE MATERIAL FOR PERMANENT MAGNET AND METHOD FOR MANUFACTURING THE SAME
CN103626483A (en) * 2013-11-29 2014-03-12 宁波科星材料科技有限公司 Praseodymium-zirconium ferrite material
CN105330282A (en) * 2015-11-27 2016-02-17 全椒君鸿软磁材料有限公司 Preparation method of high frequency low loss soft magnetic ferrite core material
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