CN113004031A - Microwave ferrite material and preparation and application method thereof - Google Patents

Microwave ferrite material and preparation and application method thereof Download PDF

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CN113004031A
CN113004031A CN202110416802.0A CN202110416802A CN113004031A CN 113004031 A CN113004031 A CN 113004031A CN 202110416802 A CN202110416802 A CN 202110416802A CN 113004031 A CN113004031 A CN 113004031A
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许方
胡建波
刘永刚
韩亚东
杨云帆
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Southwest University of Science and Technology
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Abstract

The invention discloses a microwave ferrite material and preparation and application methods thereof, belonging to the technical field of magnetic materials. The microwave ferrite material comprises the following raw material components in percentage by mass: 98.6-99.6% of Li0.43Zn0.27Ti0.13Fe2.17O40.38 to 0.42% of Nb2O5And 0.0 to 1.0% of LMZBS glass. The LiZnTi ferrite material obtained by the invention can be sintered and prepared at low temperature (900-940 ℃), has low sintering temperature, compact microstructure, low ferromagnetic resonance line width and high saturation magnetization, and can be used as an excellent LTCC phase shifter material.

Description

Microwave ferrite material and preparation and application method thereof
Technical Field
The invention relates to the technical field of microwave ferrite materials, in particular to the technical field of microwave ferrite materials applied to LTCC devices.
Background
The phase shifter is also one of the most important components in a 5G radio frequency unit as a microwave network module for providing a controllable phase difference for radio frequency signals. In recent years, electronic information technology is continuously developing towards high frequency and miniaturization, and the integration and modularization of components are more and more urgent. The ferrite green ceramic material tape based on the low temperature co-fired ceramic (LTCC) technology can be used as a ceramic substrate to manufacture various microwave passive devices, and active devices such as an IC chip, an amplifier and the like can be integrated on the surface of the ferrite green ceramic material tape, so that a passive/active integrated module is formed. The LTCC technology requires that the co-firing temperature of the ferrite is lower than the melting point (961 ℃) of the silver electrode, but the sintering temperature of the high-performance microwave ferrite prepared by the traditional method is far higher than the temperature and reaches 1100-1300 ℃. Therefore, it is an urgent technical problem to reduce the sintering temperature of microwave ferrite while maintaining excellent gyromagnetic properties and microstructure.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the microwave ferrite which can obtain high squareness ratio, high saturation magnetization and low ferromagnetic resonance line width under low-temperature sintering, and further provides a preparation method of the microwave ferrite and application of the microwave ferrite in an LTCC phase shifter.
The invention firstly provides the following technical scheme:
a microwave ferrite material comprises the following raw material components in percentage by mass: 98.6 to 99.6% of a main component, 0.38 to 0.42% of a first additive component and 0.0 to 1.0% of a second additive component, wherein the main component is a compound Li0.43Zn0.27Ti0.13Fe2.17O4The first additive component is a compound Nb2O5And the second additive component is LMZBS glass.
Wherein the LMZBS glass is Li2CO3-MgO-ZnO-B2O3-SiO2And (3) glass.
According to some preferred embodiments of the invention, the LMZBS glass is composed of LMZBS starting component Li in a molar ratio of 1:1:1:1:12CO3、MgO、ZnO、B2O3And SiO2And (4) preparing.
According to some preferred embodiments of the present invention, the main component is composed of main component raw material components Li satisfying a stoichiometric ratio of a molecular formula thereof2CO3、ZnO、TiO2And Fe2O3And (4) preparing.
The invention further provides a preparation method of the microwave ferrite material, which comprises the following steps:
mixing the powder of the first addition component, the powder of the second addition component and the main component according to the proportion to obtain mixed powder;
ball-milling the mixed powder for 5.5-6.5 hours under the ball-milling condition of 200-300 r/min until all components are uniformly mixed, and then drying to obtain ball-milled mixed powder;
adding an adhesive into the mixed powder after ball milling, and pressing into a blank;
and sintering the blank body at 900-940 ℃ for 3.5-4.5 hours, then cooling to 590-610 ℃ at a cooling rate of 1.5-2.5 ℃/min, and naturally cooling to room temperature to obtain the microwave ferrite material.
In the above scheme, the ratio is as follows: the microwave ferrite comprises the following raw materials: 98.6 to 99.6% of a main component, 0.38 to 0.42% of a first additive component, and 0.0 to 1.0% of a second additive component.
According to some preferred embodiments of the present invention, in the wet ball milling, the mass ratio of the mixed powder to water and the iron balls for grinding is 1:1: 3.
According to some preferred embodiments of the invention, the binder is polyvinyl alcohol.
According to some preferred embodiments of the present invention, the pressing pressure is 15 to 20 Mpa.
According to some preferred embodiments of the invention, the preparation of the main ingredient comprises:
mixing Li as main component2CO3ZnO and TiO2Proportioning according to the stoichiometric ratio of the molecular formula of the main component, and simultaneously adding the raw material Fe according to the iron-deficiency formula2O3Obtaining powder of a main formula;
carrying out wet ball milling on the main formula powder, and then drying to obtain a main formula mixture;
and (3) heating the mixture of the main formula to 790-830 ℃ at a heating rate of 1.5-2.5 ℃/min, preserving the heat for 2-4 hours, then cooling to 595-605 ℃ at a rate of 1.5-2.5 ℃/min, and naturally cooling to room temperature to obtain the main component.
According to some preferred embodiments of the present invention, the iron deficiency formulation has an iron deficiency of 5-8% by mass.
According to some preferred embodiments of the invention, the mass ratio of the main formula powder to water and the iron balls for grinding in wet ball milling of the main formula powder is 1 (1.5-2.0): 3.
According to some preferred embodiments of the present invention, the ball milling speed of the wet ball milling of the main formula powder is 200-.
According to some preferred embodiments of the invention, the preparation of the powder of the second additional ingredient comprises:
adding Li as a raw material of a second additive component2CO3、MgO、ZnO、B2O3And SiO2Preparing materials according to the molar ratio of 1:1:1:1:1, and then performing wet ball milling and drying to obtain a second additive component mixed powder; and raising the temperature of the second additive component mixed powder to 1200-1300 ℃ at a heating rate of 1.5-2.5 ℃/min, preserving the heat for 3.5-4.5 hours, then cooling to 990-1010 ℃, pouring into water for rapid quenching to obtain transparent glass, and drying, grinding and sieving the obtained transparent glass to obtain the second additive component powder.
The invention also discloses the application of the microwave ferrite material and/or the microwave ferrite material prepared by the preparation method in a low-temperature co-fired ceramic phase shifter.
The invention has the following beneficial effects:
the microwave ferrite material can be used for an LTCC phase shifter, and high-melting-point Nb with a fixed proportion is added into a LiZnTi microwave ferrite material2O5On the premise of not deteriorating the magnetic performance, the low-temperature sintering of the ferrite is realized by regulating and controlling the proportion of the LMZBS glass phase additive. Wherein the LMZSB glass phase additive can promote the low-temperature growth of ferrite grains through the action of liquid phase, and Nb2O5Can prevent the abnormal growth of crystal grains, and can promote the uniform and compact growth of the ferrite at low temperature under the synergistic action of the crystal grains and the ferrite to obtain the LiZnTi ferrite material with excellent performance.
The invention adds Nb with specific proportion2O5And the LMZBS glass phase can reduce the sintering temperature of the obtained LiZnTi ferrite material from 1200 ℃ to 900-940 ℃, and abnormal large grains are not generated while high squareness ratio, high saturation magnetization and low ferromagnetic resonance line width are maintained.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) comparison of ferrite obtained in example 3 of the present invention and a comparative example, wherein a is an SEM image of the ferrite material obtained in example 3, and b is an SEM image of the ferrite material obtained in the comparative example.
Detailed Description
The present invention is described in detail below with reference to the following embodiments and the attached drawings, but it should be understood that the embodiments and the attached drawings are only used for the illustrative description of the present invention and do not limit the protection scope of the present invention in any way. All reasonable variations and combinations that fall within the spirit of the invention are intended to be within the scope of the invention.
According to the technical scheme of the invention, some specific embodiments are as follows:
a microwave ferrite material for LTCC phase shifter is composed of 98.6-99.6 wt% of main formula and 0.4 wt% of composite additive2O5And 0.0 to 1.0 percent of Li2CO3-MgO-ZnO-B2O3-SiO2(LMZBS) glass, the main formula of the microwave ferrite is Li0.43Zn0.27Ti0.13Fe2.17O4The LMZBS glass is prepared from raw materials according to a molar ratio Li2CO3:MgO:ZnO:B2O3:SiO2The configuration is 1:1:1:1: 1.
Wherein the LMZBS glass can be further obtained by the following embodiments: ball-milling, drying and sieving the LMZBS glass raw material, then heating to 1200-1350 ℃ in a sintering furnace, preserving the heat for 2-4 hours, cooling to 1000 ℃, adding into room temperature deionized water, and rapidly quenching to obtain the LMZBS glass.
The preparation method can further comprise the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Starting material, i.e. Fe by less than calculation2O3Mass to Fe2O3The raw materials are dosed, preferably in a calculated amount of 92-95 wt% for Fe2O3Weighing and preparing to obtain main formula powder;
step 2: according to the obtained main formula, the powder material: deionized water: performing primary ball milling and mixing on the powder of the main formula according to the mass ratio of (1.5-2.0) to (3), wherein the ball milling time is 3.5-4.5 hours, the ball milling rotating speed is 200-300 r/min, drying the powder in an oven after ball milling, putting the powder into a sintering furnace for presintering treatment, raising the temperature to 790-830 ℃ at the heating rate of 1.5-2.5 ℃/min, preserving the heat for 2-4 hours, then cooling to 595-605 ℃ at the speed of 1.5-2.5 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi main material;
and step 3: with Li2CO3、MgO、ZnO、B2O3、SiO2As raw materials, the raw materials are mixed according to the mol ratio Li2CO3:MgO:ZnO:B2O3:SiO2Proportioning according to the proportion of 1:1:1:1: 1:1, ball-milling for 7.5-8.5 hours by a wet method, drying the mixture in an oven, grinding, sieving, transferring the powder into an alumina crucible, placing in a sintering furnace, heating to 1200-1300 ℃ at the heating rate of 1.5-2.5 ℃/min, preserving heat for 3.5-4.5 hours,cooling to 990-;
and 4, step 4: mixing Nb with2O5Mixing the obtained LMZBS glass obtained in the step 3 with the LiZnTi main material obtained in the step 2 to prepare powder, wherein the mass percent of the main material is 98.6-99.6%, and Nb is2O50.4 percent of LMZBS glass and 0.0-1.0 percent of LMZBS glass by mass percent, and carrying out secondary ball milling on the mixed powder, wherein the powder comprises the following components in percentage by mass: deionized water: the iron ball is 1:1:3, the ball milling time is 5.5-6.5 hours, and the ball milling rotating speed is 200-; and then taking out the mixture for drying, adding a polyvinyl alcohol (PVA) adhesive for granulation molding and pressing into a blank, then placing the blank into a sintering furnace, sintering for 3.5-4.5 hours at the temperature of 900-940 ℃, then cooling to 590-610 ℃ at the speed of 1.5-2.5 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi microwave ferrite material.
Wherein, in the iron deficiency formula in the step 1, the mass percentage of the iron deficiency can be 5-8%.
And furthermore, when the blank is pressed in the step 4, the pressure can be 15-20 MPa.
According to the above-mentioned embodiments, the present invention further provides the following examples:
example 1
A preparation method of a microwave ferrite material for an LTCC phase shifter comprises the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Preparing raw materials to obtain main formula powder;
step 2: the powder material comprises the following components in percentage by mass: deionized water: carrying out primary ball milling mixing on iron balls according to the proportion of 1:1.5:3, wherein the ball milling time is 4 hours, the ball milling rotating speed is 250 revolutions per minute, drying the powder in an oven after ball milling, putting the obtained powder into a sintering furnace for presintering treatment, raising the temperature to 800 ℃ at the rate of 2 ℃/minute, keeping the temperature for 2 hours, then reducing the temperature to 600 ℃ at the rate of-2 ℃/minute, and then naturally reducing the temperature to room temperature to obtain a LiZnTi main material;
and step 3: with Li2CO3、MgO、ZnO、B2O3、SiO2As raw materials, the raw materials are mixed according to the mol ratio Li2CO3:MgO:ZnO:B2O3:SiO2Proportioning according to the proportion of 1:1:1:1: 1:1, carrying out wet ball milling for 8 hours, drying the mixture in an oven, grinding and sieving, then transferring the powder into an alumina crucible, placing the alumina crucible in a sintering furnace, raising the temperature to 1250 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 4 hours, cooling to 1000 ℃, pouring the cooled powder into deionized water, carrying out rapid quenching to obtain transparent glass, drying, grinding and sieving with a 200-mesh sieve to obtain the LMZBS glass additive;
and 4, step 4: nb in percentage by mass2O5Mixing the LMZBS glass obtained in the step 3 with the LiZnTi main material obtained in the step 2 to prepare powder, wherein the mass percent of the main material is 99.6 percent, and Nb is added2O50.4 percent of LMZBS glass and 0.0 percent of LMZBS glass by mass percent, and carrying out secondary ball milling, wherein the weight percentage of the powder is as follows: deionized water: the iron ball is 1:1:3, the ball milling time is 6 hours, and the ball milling speed is 250 r/min; and then taking out the mixture for drying, adding a polyvinyl alcohol (PVA) adhesive for granulation and molding, pressing into a blank body, putting the blank body into a sintering furnace, sintering for 4 hours at the temperature of 900 ℃, then cooling to 600 ℃ at the speed of-2 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi microwave ferrite material.
The LiZnTi microwave ferrite material is tested by testing means such as a B-H analyzer, a vibration sample magnetometer and a drainage method, and the results are as follows:
density of the sample: 4.19g/cm3(ii) a Saturation magnetization: 3331.3 Gs; coercive force: 12.1 Oe; saturation magnetic induction: 224.6 mT; rectangle ratio: 0.849.
example 2
A preparation method of a microwave ferrite material for an LTCC phase shifter comprises the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Preparing raw materials to obtain main formula powder;
step 2: the powder material comprises the following components in percentage by mass: deionized water: carrying out primary ball milling mixing on iron balls according to the proportion of 1:1.5:3, wherein the ball milling time is 4 hours, the ball milling rotating speed is 250 revolutions per minute, drying the powder in an oven after ball milling, putting the obtained powder into a sintering furnace for presintering treatment, raising the temperature to 800 ℃ at the rate of 2 ℃/minute, keeping the temperature for 2 hours, then reducing the temperature to 600 ℃ at the rate of-2 ℃/minute, and then naturally reducing the temperature to room temperature to obtain a LiZnTi main material;
and step 3: with Li2CO3、MgO、ZnO、B2O3、SiO2As raw materials, the raw materials are mixed according to the mol ratio Li2CO3:MgO:ZnO:B2O3:SiO2Proportioning according to the proportion of 1:1:1:1: 1:1, carrying out wet ball milling for 8 hours, drying the mixture in an oven, grinding and sieving, then transferring the powder into an alumina crucible, placing the alumina crucible in a sintering furnace, raising the temperature to 1250 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 4 hours, cooling to 1000 ℃, pouring the cooled powder into deionized water, carrying out rapid quenching to obtain transparent glass, drying, grinding and sieving with a 200-mesh sieve to obtain the LMZBS glass additive;
and 4, step 4: nb in percentage by mass2O5Mixing the LMZBS glass obtained in the step 3 with the LiZnTi main material obtained in the step 2 to prepare powder, wherein the mass percent of the main material is 99.35 percent, and Nb is added2O5The mass percent is 0.4%, the mass percent of LMZBS glass is 0.25%, and secondary ball milling is carried out, wherein, the powder: deionized water: the iron ball is 1:1:3, the ball milling time is 6 hours, and the ball milling speed is 250 r/min; then taking out the mixture to dry, adding polyvinyl alcohol (PVA) adhesive to granulate and form and press the mixture into a blank body, then putting the blank body into a sintering furnace to sinter for 4 hours at the temperature of 900 ℃, and then sintering the blank body for 2 ℃ below zeroCooling to 600 ℃ at a speed of 600 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi microwave ferrite material.
The LiZnTi microwave ferrite material obtained in the present example was tested by the same method as in example 1, and the results thereof were as follows: density of the sample: 4.61g/cm3(ii) a Saturation magnetization: 3607.3 Gs; coercive force: 2.4 Oe; saturation magnetic induction: 278.9 mT; rectangle ratio: 0.853.
example 3
A preparation method of a microwave ferrite material for an LTCC phase shifter comprises the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Preparing raw materials to obtain main formula powder;
step 2: the powder material comprises the following components in percentage by mass: deionized water: carrying out primary ball milling mixing on iron balls according to the proportion of 1:1.5:3, wherein the ball milling time is 4 hours, the ball milling rotating speed is 250 revolutions per minute, drying the powder in an oven after ball milling, putting the obtained powder into a sintering furnace for presintering treatment, raising the temperature to 800 ℃ at the rate of 2 ℃/minute, keeping the temperature for 2 hours, then reducing the temperature to 600 ℃ at the rate of-2 ℃/minute, and then naturally reducing the temperature to room temperature to obtain a LiZnTi main material;
and step 3: with Li2CO3、MgO、ZnO、B2O3、SiO2As raw materials, the raw materials are mixed according to the mol ratio Li2CO3:MgO:ZnO:B2O3:SiO2Proportioning according to the proportion of 1:1:1:1: 1:1, carrying out wet ball milling for 8 hours, drying the mixture in an oven, grinding and sieving, then transferring the powder into an alumina crucible, placing the alumina crucible in a sintering furnace, raising the temperature to 1250 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 4 hours, cooling to 1000 ℃, pouring the cooled powder into deionized water, carrying out rapid quenching to obtain transparent glass, drying, grinding and sieving with a 200-mesh sieve to obtain the LMZBS glass additive;
and 4, step 4: nb in percentage by mass2O5Mixing the LMZBS glass obtained in the step 3 with the LiZnTi main material obtained in the step 2 to prepare powder, wherein the mass percent of the main material is 99.1 percent, and Nb is added2O5The mass percent is 0.4%, the mass percent of LMZBS glass is 0.5%, and secondary ball milling is carried out, wherein, the powder: deionized water: the iron ball is 1:1:3, the ball milling time is 6 hours, and the ball milling speed is 250 r/min; and then taking out the mixture for drying, adding a polyvinyl alcohol (PVA) adhesive for granulation and molding, pressing into a blank body, putting the blank body into a sintering furnace, sintering for 4 hours at the temperature of 900 ℃, then cooling to 600 ℃ at the speed of-2 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi microwave ferrite material.
The LiZnTi microwave ferrite material prepared in the example 3 is tested by the same test method as the example 1, and the performance of the LiZnTi microwave ferrite material is as follows: density of the sample: 4.62g/cm3(ii) a Saturation magnetization: 3719.5 Gs; coercive force: 1.7 Oe; saturation magnetic induction: 294.2 mT; rectangle ratio: 0.874.
example 4
A preparation method of a microwave ferrite material for an LTCC phase shifter comprises the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Preparing raw materials to obtain main formula powder;
step 2: the powder material comprises the following components in percentage by mass: deionized water: carrying out primary ball milling mixing on iron balls according to the proportion of 1:1.5:3, wherein the ball milling time is 4 hours, the ball milling rotating speed is 250 revolutions per minute, drying the powder in an oven after ball milling, putting the obtained powder into a sintering furnace for presintering treatment, raising the temperature to 800 ℃ at the rate of 2 ℃/minute, keeping the temperature for 2 hours, then reducing the temperature to 600 ℃ at the rate of-2 ℃/minute, and then naturally reducing the temperature to room temperature to obtain a LiZnTi main material;
and step 3: with Li2CO3、MgO、ZnO、B2O3、SiO2Is used as a raw material for preparing the high-purity,raw materials are mixed according to the mol ratio Li2CO3:MgO:ZnO:B2O3:SiO2Proportioning according to the proportion of 1:1:1:1: 1:1, carrying out wet ball milling for 8 hours, drying the mixture in an oven, grinding and sieving, then transferring the powder into an alumina crucible, placing the alumina crucible in a sintering furnace, raising the temperature to 1250 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 4 hours, cooling to 1000 ℃, pouring the cooled powder into deionized water, carrying out rapid quenching to obtain transparent glass, drying, grinding and sieving with a 200-mesh sieve to obtain the LMZBS glass additive;
and 4, step 4: nb in percentage by mass2O5Mixing the obtained LMZBS glass obtained in the step 3, adding the mixture into the LiZnTi main material obtained in the step 2 to prepare powder, wherein the mass percent of the main material is 98.85%, and Nb is2O50.4 percent by mass and 0.75 percent by mass of LMZBS glass, and carrying out secondary ball milling, wherein the weight percentage of the powder material is as follows: deionized water: the iron ball is 1:1:3, the ball milling time is 6 hours, and the ball milling speed is 250 r/min; and then taking out the mixture for drying, adding a polyvinyl alcohol (PVA) adhesive for granulation and molding, pressing into a blank body, putting the blank body into a sintering furnace, sintering for 4 hours at the temperature of 900 ℃, then cooling to 600 ℃ at the speed of-2 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi microwave ferrite material.
The LiZnTi microwave ferrite material prepared in the example 4 is tested by the same test method as the example 1, and the performance of the LiZnTi microwave ferrite material is as follows: density of the sample: 4.61g/cm3(ii) a Saturation magnetization: 3670.9 Gs; coercive force: 6.9 Oe; saturation magnetic induction: 290.9 mT; rectangle ratio: 0.864.
example 5
A preparation method of a microwave ferrite material for an LTCC phase shifter comprises the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Preparing raw materials to obtain main formula powder;
step 2: the powder material comprises the following components in percentage by mass: deionized water: carrying out primary ball milling mixing on iron balls according to the proportion of 1:1.5:3, wherein the ball milling time is 4 hours, the ball milling rotating speed is 250 revolutions per minute, drying the powder in an oven after ball milling, putting the obtained powder into a sintering furnace for presintering treatment, raising the temperature to 800 ℃ at the rate of 2 ℃/minute, keeping the temperature for 2 hours, then reducing the temperature to 600 ℃ at the rate of-2 ℃/minute, and then naturally reducing the temperature to room temperature to obtain a LiZnTi main material;
and step 3: with Li2CO3、MgO、ZnO、B2O3、SiO2As raw materials, the raw materials are mixed according to the mol ratio Li2CO3:MgO:ZnO:B2O3:SiO2Proportioning according to the proportion of 1:1:1:1: 1:1, carrying out wet ball milling for 8 hours, drying the mixture in an oven, grinding and sieving, then transferring the powder into an alumina crucible, placing the alumina crucible in a sintering furnace, raising the temperature to 1250 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 4 hours, cooling to 1000 ℃, pouring the cooled powder into deionized water, carrying out rapid quenching to obtain transparent glass, drying, grinding and sieving with a 200-mesh sieve to obtain the LMZBS glass additive;
and 4, step 4: nb in percentage by mass2O5Mixing the obtained LMZBS glass obtained in the step 3, adding the mixture into the LiZnTi main material obtained in the step 2 to prepare powder, wherein the mass percent of the main material is 98.6%, and Nb is2O5The mass percent of the LMZBS glass is 0.4%, the mass percent of the LMZBS glass is 1.0%, and secondary ball milling is carried out, wherein the powder material: deionized water: the iron ball is 1:1:3, the ball milling time is 6 hours, and the ball milling speed is 250 r/min; and then taking out the mixture for drying, adding a polyvinyl alcohol (PVA) adhesive for granulation and molding, pressing into a blank body, putting the blank body into a sintering furnace, sintering for 4 hours at the temperature of 900 ℃, then cooling to 600 ℃ at the speed of-2 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi microwave ferrite material.
The LiZnTi microwave ferrite material prepared in the example 5 has the following properties by the same test method as the example 1: density of the sample: 4.47g/cm3(ii) a Saturation magnetization: 3643.7 Gs; coercive force: 5.8 Oe; saturation magnetic induction: 264.3 mT; rectangle ratio: 0.852.
comparative example
A preparation method of a microwave ferrite material for an LTCC phase shifter comprises the following steps:
step 1: with Li2CO3、ZnO、TiO2、Fe2O3As starting material, according to Li0.43Zn0.27Ti0.13Fe2.17O4Calculating the proportion of molecular formula, and weighing Fe by adopting iron deficiency formula2O3Preparing raw materials to obtain main formula powder;
step 2: the powder material comprises the following components in percentage by mass: deionized water: carrying out primary ball milling mixing on iron balls according to the proportion of 1:1.5:3, wherein the ball milling time is 4 hours, the ball milling rotating speed is 250 revolutions per minute, drying the powder in an oven after ball milling, putting the obtained powder into a sintering furnace for presintering treatment, raising the temperature to 800 ℃ at the rate of 2 ℃/minute, keeping the temperature for 2 hours, then reducing the temperature to 600 ℃ at the rate of-2 ℃/minute, and then naturally reducing the temperature to room temperature to obtain a LiZnTi main material;
and step 3: and (3) carrying out secondary ball milling on the LiZnTi main material obtained in the step (2), wherein the powder material comprises the following components: deionized water: the iron ball is 1:1:3, the ball milling time is 6 hours, and the ball milling speed is 250 r/min; and then taking out the mixture for drying, adding a polyvinyl alcohol (PVA) adhesive for granulation and molding, pressing into a blank, putting the blank into a sintering furnace, sintering for 4 hours at the temperature of 900 ℃, then cooling to 600 ℃ at the speed of-2 ℃/min, and then naturally cooling to room temperature to obtain the LiZnTi contrast microwave ferrite material.
The LiZnTi microwave ferrite material prepared by the comparative example is tested by the same test method as the example 1, and has the following properties: density of the sample: 3.83g/cm3(ii) a Saturation magnetization: 3069.1 Gs; coercive force: 15.9 Oe; saturation magnetic induction: 199.2 mT; rectangle ratio: 0.784.
the product of the comparative example was compared with the LiZnTi ferrite material obtained in example 3 in microstructure, and SEM images of the two were shown in FIG. 1. As can be seen from FIG. 1, example 3 was obtained by adding Nb in a fixed ratio of 0.4%2O5And 0.5% of LMZBS glass additiveThe grains are obviously grown and have compact structure, and no obvious abnormal large grains appear. The comparison of the magnetic parameter test results can also show that the LiZnTi ferrite prepared by the method not only has obviously increased saturation magnetization, but also has low coercive force and high squareness ratio.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.

Claims (10)

1. A microwave ferrite material, characterized by: the material comprises the following raw material components in percentage by mass: 98.6 to 99.6% of a main component, 0.38 to 0.42% of a first additive component and 0.0 to 1.0% of a second additive component, wherein the main component is a compound Li0.43Zn0.27Ti0.13Fe2.17O4The first additive component is a compound Nb2O5And the second additive component is LMZBS glass.
2. A microwave ferrite material in accordance with claim 1, wherein: the LMZBS glass consists of LMZBS raw material component Li in a molar ratio of 1:1:1:1:12CO3、MgO、ZnO、B2O3And SiO2And (4) preparing.
3. A microwave ferrite material in accordance with claim 1, wherein: the main component is composed of a main component raw material component Li satisfying the stoichiometric ratio of the molecular formula2CO3、ZnO、TiO2And Fe2O3And (4) preparing.
4. A method of preparing a microwave ferrite material as claimed in any of claims 1 to 3, characterized in that: the method comprises the following steps:
mixing the powder of the first addition component, the powder of the second addition component and the main component according to the proportion to obtain mixed powder;
carrying out wet ball milling on the mixed powder for 5.5-6.5 hours under the ball milling condition of 200-300 revolutions per minute, and then drying to obtain ball-milled mixed powder;
adding an adhesive into the mixed powder after ball milling, and pressing into a blank;
and sintering the blank body at 900-940 ℃ for 3.5-4.5 hours, then cooling to 590-610 ℃ at a cooling rate of 1.5-2.5 ℃/min, and naturally cooling to room temperature to obtain the microwave ferrite material.
5. The method of claim 4, wherein: in the wet ball milling, the mass ratio of the mixed powder to water and the iron balls for grinding is 1:1: 3.
6. The method of claim 4, wherein: and adding the mixed powder after ball milling into the adhesive to press to obtain the blank, wherein the adhesive is polyvinyl alcohol, and/or the pressing pressure is 15-20 Mpa.
7. The method of claim 4, wherein: the preparation of the main component comprises the following steps:
mixing Li as main component2CO3ZnO and TiO2Proportioning according to the stoichiometric ratio of the molecular formula of the main component, and simultaneously adding the raw material Fe according to the iron-deficiency formula2O3Obtaining powder of a main formula;
carrying out wet ball milling on the main formula powder, and then drying to obtain a main formula mixture;
and (3) heating the mixture of the main formula to 790-830 ℃ at a heating rate of 1.5-2.5 ℃/min, preserving the heat for 2-4 hours, then cooling to 595-605 ℃ at a rate of 1.5-2.5 ℃/min, and naturally cooling to room temperature to obtain the main component.
8. The method of claim 7, wherein: in the preparation of the main component, the mass percentage of iron deficiency in the iron deficiency formula is 5-8%; and/or in the wet ball milling of the main formula powder, the mass ratio of the main formula powder to water and iron balls for grinding is 1 (1.5-2.0): 3; and/or the ball milling rotation speed of the wet ball milling of the main formula powder is 200-300 r/min; and/or the ball milling time of the wet ball milling of the powder of the main formula is 3.5-4.5 hours.
9. The method of claim 4, wherein: the preparation of the powder of the second additive component comprises the following steps:
adding Li as a raw material of a second additive component2CO3、MgO、ZnO、B2O3And SiO2Preparing materials according to the molar ratio of 1:1:1:1:1, and then performing wet ball milling and drying to obtain a second additive component mixed powder; and raising the temperature of the second additive component mixed powder to 1200-1300 ℃ at a heating rate of 1.5-2.5 ℃/min, preserving the heat for 3.5-4.5 hours, then cooling to 990-1010 ℃, pouring into water for rapid quenching to obtain transparent glass, and drying, grinding and sieving the obtained transparent glass to obtain the second additive component powder.
10. Use of the microwave ferrite material according to any one of claims 1 to 3 and/or the microwave ferrite material prepared by the preparation method according to any one of claims 4 to 9 in a low temperature co-fired ceramic phase shifter.
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