CN114213115B - Microwave dielectric material and preparation method thereof - Google Patents
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Abstract
The invention discloses a microwave dielectric ceramic material and a preparation method thereof, belonging to electronic information functional ceramics and electronic devicesThe technical field of the device. The composition expression of the microwave dielectric ceramic material is as follows: mg (magnesium) 2.1 Al 4 Si 5 O 18 ‑xMg m Ti n O y Wherein: x is more than or equal to 0.2 and less than or equal to 1.0. By introducing Mg-Ti series oxide, the sintering temperature is successfully reduced to 1280-1310 ℃, and the density of the obtained porcelain body is 2.42-2.66 g/cm 3 The dielectric constant of the microwave dielectric ceramic material is 5.0 to 5.8, the Qxf value is 51674 to 69974GHz, and the frequency temperature coefficient tau f Is-29.5 to-24.8 ppm/DEG C, and the adhesive force of the silver layer after the metallization of the porcelain body is 10.2 to 15.6N/mm 2 。
Description
Technical Field
The invention relates to the technical field of electronic information functional ceramics and electronic devices, in particular to a microwave dielectric ceramic material and a preparation method thereof.
Background
The microwave dielectric ceramic material is a ceramic material which is applied to a wave band of 300 MHz-300 GHz as a dielectric material and can complete one or more functions, is widely applied to microwave components such as resonators, filters, capacitors, dielectric waveguide loops and the like in modern communication, and is an indispensable core material for different applications such as millimeter wave communication, electronic circuit packaging, dielectric resonant antennas, base station communication, miniaturized mobile communication and the like.
The ceramic material with low dielectric constant and high quality factor is mainly applied to the manufacturing occasions of microwave or millimeter wave electronic equipment, and comprises components with resonant frequency of 1-40 GHz, such as ceramic capacitors, various filters, duplexers, resonators and the like, for example, millimeter wave dielectric ceramics has wider application space than Surface Acoustic Wave (SAW) filters and film bulk acoustic wave (FBAR) filters with the use frequency limited to 5-10 GHz. Low microwave dielectric constant (epsilon) r ) Ceramics are also potential information memory materials of dynamic random access memories, gate dielectric materials of field effect transistor logic components and complementary metal oxide semiconductors. The low dielectric microwave dielectric ceramic is widely applied to high-end millimeter wave microwave devices such as satellite communication, GPS (global positioning system) antennas and the like. The size of the dielectric constant influences the speed of signal transmission, the low dielectric constant can reduce the interactive coupling effect of electromagnetic signals and improve the signal transmission and response speed, and the lower the dielectric constant, the smaller the signal transmission delay; high quality factor (Q) can reduce energy consumption during signal transmission, and increase deviceFrequency selectivity of the device. Therefore, in high frequency signal systems, low dielectric constant ceramic materials are of great importance to reduce signal delay.
In the existing research and industrial application, the low dielectric constant microwave dielectric material system with the dielectric constant of less than 10 is mainly binary or ternary silicate, and the typical representative of the low dielectric constant microwave dielectric material system is Zn/Mg 2 SiO 4 、Re 2 SiO 5 、CaSiO 3 Cordierite Mg 2 Al 4 Si 5 O 18 Leptopside type ABC 2 O 6 Akermanite type A 2 BC 2 O 7 And a type of square column stone A 2 BSi 2 O 7 And so on. Wherein cordierite-based Mg 2 Al 4 Si 5 O 18 The materials have been studied by several scholars in recent years due to their lower dielectric constant and near-zero coefficient of thermal expansion, such as Song and others which propose Mg 2 Al 4 Si 5 O 18 +TiO 2 The material system (sintering temperature is 1350-1450 ℃), (1-x) Mg is proposed by Susan et al 2 Al 4 Si 5 O 18 -xMg 2 SiO 4 The material system (sintering temperature is 1420-1500 ℃), and the like, and provides (100-x) wt% Mg 2 Al 4 Si 5 O 18 -x wt％Zr 0.6 Sn 0.4 TiO 4 The material system (sintering temperature is 1400 ℃).
The cordierite based Mg 2 Al 4 Si 5 O 18 The sintering temperature of the material is too high and is close to the melting temperature of cordierite at 1450-1500 ℃, and the cordierite with a hollow six-membered ring structure is difficult to obtain ceramic materials with high enough densification degree (single-phase cordierite is more applied to the fields of high-temperature refractory materials, honeycomb ceramic materials and the like), so that the adhesive force after the combination of ceramic and metal is influenced, and the application of the material in the field of electronic ceramic components with surface metallization requirements is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a microwave dielectric ceramic material with reduced sintering temperature and higher ceramic density and a preparation method thereof, and the sintering of the microwave dielectric ceramic materialThe forming temperature is reduced to 1280 to 1310 ℃, and the density of the obtained porcelain body is 2.42 to 2.66g/cm 3 Dielectric constant of 5.0-5.8, Q x f (Q is quality factor of material, f is resonance frequency) value of 51674-69974 GHz, and frequency temperature coefficient tau f Is-29.5 to-24.8 ppm/DEG C, and the adhesive force of the silver layer is 10.2 to 15.6N/mm 2 。
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a microwave dielectric ceramic material has a composition expression as follows: mg (magnesium) 2.1 Al 4 Si 5 O 18 -xMg m Ti n O y Wherein: x is more than or equal to 0.2 and less than or equal to 1.0 m Ti n O y Is MgTiO 3 、Mg 2 TiO 4 Or MgTi 2 O 5 。
The sintering temperature of the microwave dielectric ceramic material is 1280-1310 ℃.
The ceramic density of the microwave dielectric ceramic material is 2.42-2.66 g/cm 3 。
The dielectric constant of the microwave dielectric ceramic material is 5.0-5.8, the Qxf value is 51674-69974 GHz, and the frequency temperature coefficient tau f Is-29.5 to-24.8 ppm/DEG C.
The adhesive force of the silver layer of the microwave dielectric ceramic material is 10.2-15.6N/mm 2 。
When x =0.6, the dielectric constant of the microwave dielectric ceramic material is 5.3, the Q x f value is 69974GHz, and the frequency temperature coefficient tau is f Is-25.9 ppm/DEG C, the sintering temperature is 1300 ℃, and the adhesive force of the silver layer is 15.6N/mm 2 。
The preparation method of the microwave dielectric ceramic material specifically comprises the following steps:
(1) Preparing materials: firstly, weighing magnesium oxide, aluminum oxide, silicon dioxide and titanium dioxide according to a composition expression of the microwave dielectric ceramic material, and uniformly mixing to obtain a mixture;
(2) Mixing: performing ball milling treatment on the mixture obtained in the step (1) and drying to obtain dry powder;
(3) Pre-burning: placing the obtained dry powder in an alumina crucible, and presintering in a carbon rod furnace to obtain pre-synthesized powder;
(4) Pulping: ball-milling and crushing the pre-synthesized powder for 20-26 hours, wherein ball-milling media are zirconium balls and deionized water to obtain viscous slurry;
(5) Molding: and (4) adding a binder which accounts for 5-20 wt% of the weight of the slurry into the slurry obtained in the step (4), then sequentially carrying out spray granulation and compression molding, and finally sintering and molding in a carbon rod furnace to obtain the microwave dielectric ceramic material.
In the step (2), in the ball milling process, the ball milling medium is zirconium balls and deionized water; after ball milling, the mixture is placed in an oven at 150 ℃ and dried for 12 hours.
In the step (3), presintering is carried out in a carbon rod furnace at the temperature of 1000-1150 ℃ for 2-4 hours.
In the step (5), the sintering temperature is 1280-1310 ℃ in a carbon rod furnace, and the sintering time is 3 hours.
The invention has the following advantages and beneficial effects:
1. the invention designs Mg 2.1 Al 4 Si 5 O 18 -xMg m Ti n O y The cordierite matrix is designed for the non-stoichiometric ratio of Mg (increased by 0.1 mol), and 0.2-1.0 mol of Mg is introduced m Ti n O y Temperature and Mg for sintering a Material System into porcelain 2 Al 4 Si 5 O 18 The melting temperature is pulled open, the sintering temperature is reduced to 1280-1310 ℃, the density of the porcelain body is improved, and the requirement of silver layer adhesive force applied to the electronic ceramic component is met.
2. The microwave dielectric material of the invention ensures that the dielectric constant is kept below 6.0 and the Qf value is ensured to be above 50000GHz on the premise of ensuring the reduction of the sintering temperature, the specific dielectric constant is 5.0-5.8, the Qxf value is 51674-69974 GHz, and the frequency temperature coefficient tau f Is-29.5 to-24.8 ppm/DEG C, and can be widely applied to the fields of millimeter wave devices, baseband antennas, navigation antennas, dielectric waveguide filters and the like.
Drawings
FIG. 1 is an XRD pattern of the microwave dielectric ceramic material prepared in examples 1-7.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples.
Examples 1 to 7:
the microwave dielectric ceramic material comprises the following components in an expression formula: mg (Mg) 2.1 Al 4 Si 5 O 18 -xMg m Ti n O y Wherein: x is more than or equal to 0.2 and less than or equal to 1.0 m Ti n O y Is MgTiO 3 、Mg 2 TiO 4 Or MgTi 2 O 5 。
Examples 1-7 specific compositional proportions are shown in Table 1, wherein the Mg of examples 1-5 m Ti n O y The phase is designed to be MgTiO 3 Mg of example 6 m Ti n O y The phase is designed to be Mg 2 TiO 4 Mg of example 7 m Ti n O y The phase is designed to be MgTi 2 O 5 。
The preparation method of the microwave dielectric ceramic material comprises the following specific steps:
(1) Preparing materials: magnesium oxide, aluminum oxide, silicon dioxide and titanium dioxide are used as raw materials, and Mg is firstly used as raw material 2.1 Al 4 Si 5 O 18 -xMgTiO 3 Weighing magnesium oxide, aluminum oxide, silicon dioxide and titanium dioxide, and uniformly mixing to obtain a mixture;
(2) Mixing: performing ball milling treatment on the mixed material after burdening, wherein ball milling media are zirconium balls and deionized water; after ball milling, placing the mixture in a drying oven at 150 ℃ for drying treatment for 12 hours to obtain dry powder;
(3) Pre-burning: placing the obtained dry powder in different alumina crucibles, and presintering the dry powder in a carbon rod furnace at 1100 ℃ for 3 hours to obtain pre-synthesized powder;
(4) Pulping: ball-milling and crushing the secondary raw material powder for 20-26 hours, wherein ball-milling media are zirconium balls and deionized water to obtain viscous slurry;
(5) Molding: and (4) adding a polyvinyl alcohol binder which accounts for 10wt% of the slurry into the slurry obtained in the step (4), then sequentially carrying out spray granulation and compression molding, and finally carrying out sintering molding at 1280-1310 ℃ for 3 hours in a carbon rod furnace to obtain the microwave dielectric ceramic material.
FIG. 1 shows XRD patterns of the microwave dielectric ceramic materials of examples 1-7. As can be seen from the figure, mg after sintering into porcelain m Ti n O y The second phase is MgTi with lowest phase synthesis temperature requirement 2 O 5 The two phases exist independently, and the corresponding diffraction peaks are gradually enhanced along with the increase of the x value. MgTi after sintering into porcelain 2 O 5 The existence of the phase is the key of the material system which can reduce the sintering temperature and the porcelain forming temperature and melting temperature interval of the drawing cordierite system.
Table 1 shows the microwave dielectric properties and sintering characteristics of each constituent material of examples 1 to 7.
TABLE 1 Mg 2.1 Al 4 Si 5 O 18 -xMg m Ti n O y Dielectric property of microwave
As can be seen from Table 1, in examples 1 to 5, the present invention designed a slight excess of Mg in the cordierite main phase, corresponding to MgTiO 3 After the second phase is introduced, the sintering temperature of the material system is greatly reduced, and the density of the ceramic body is also improved. Meanwhile, the dielectric constant is not improved to be more than 6.0 under the condition of ensuring that the Q multiplied by f value is high enough, the material has low enough dielectric constant, high Q multiplied by f value and high ceramic density, and can meet the adhesive force of a silver layer of application, thereby greatly increasing the opportunity of applying the material in the fields of millimeter wave communication with higher resonant frequency, electronic circuit packaging, dielectric resonant antennas, base station communication, miniaturized mobile communication and the like. In addition, the fruitExamples 6 and 7 give x =0.6, the second phase is designed as Mg respectively 2 TiO 4 And MgTi 2 O 5 In the process, the sintering property, the dielectric property and the silver layer adhesive force of the material system can reach the design that the second phase is MgTiO 3 Similar effects apply.
Claims (8)
1. A microwave dielectric ceramic material is characterized in that: the composition expression of the microwave dielectric ceramic material is as follows: mg (magnesium) 2.1 Al 4 Si 5 O 18 -xMg m Ti n O y Wherein: x is more than or equal to 0.2 and less than or equal to 1.0 m Ti n O y Is MgTiO 3 、Mg 2 TiO 4 Or MgTi 2 O 5 ；
The sintering temperature of the microwave dielectric ceramic material is 1280-1310 ℃;
the ceramic density of the microwave dielectric ceramic material is 2.42-2.66 g/cm 3 。
2. A microwave dielectric ceramic material according to claim 1, wherein: the dielectric constant of the microwave dielectric ceramic material is 5.0-5.8, the Qxf value is 51674-69974 GHz, and the frequency temperature coefficient tau f Is-29.5 to-24.8 ppm/DEG C.
3. A microwave dielectric ceramic material according to claim 1, wherein: the adhesive force of the silver layer of the microwave dielectric ceramic material is 10.2-15.6N/mm 2 。
4. A microwave dielectric ceramic material according to claim 1 or 2, wherein: when x =0.6, the dielectric constant of the microwave dielectric ceramic material is 5.3, the Q x f value is 69974GHz, and the frequency temperature coefficient tau f Is-25.9 ppm/DEG C, the sintering temperature is 1300 ℃, and the adhesive force of the silver layer is 15.6N/mm 2 。
5. A method for preparing a microwave dielectric ceramic material as claimed in claim 1, wherein: the method specifically comprises the following steps:
(1) Preparing materials: firstly, weighing magnesium oxide, aluminum oxide, silicon dioxide and titanium dioxide according to a composition expression of the microwave dielectric ceramic material, and uniformly mixing to obtain a mixture;
(2) Mixing: performing ball milling treatment on the mixture obtained in the step (1) and drying to obtain dry powder;
(3) Pre-burning: placing the obtained dry powder in an alumina crucible, and presintering in a carbon rod furnace to obtain pre-synthesized powder;
(4) Pulping: ball-milling and crushing the pre-synthesized powder for 20-26 hours, wherein ball-milling media are zirconium balls and deionized water to obtain viscous slurry;
(5) Molding: and (4) adding a binder which accounts for 5-20 wt% of the weight of the slurry into the slurry obtained in the step (4), then sequentially carrying out spray granulation and compression molding, and finally sintering and molding in a carbon rod furnace to obtain the microwave dielectric ceramic material.
6. A method for preparing microwave dielectric ceramic material according to claim 5, characterized in that: in the step (2), in the ball milling process, a ball milling medium is zirconium balls and deionized water; after ball milling, the mixture is placed in an oven at 150 ℃ for drying treatment for 12 hours.
7. A method for preparing a microwave dielectric ceramic material as claimed in claim 5, wherein: in the step (3), presintering is carried out in a carbon rod furnace at the temperature of 1000-1150 ℃ for 2-4 hours.
8. A method for preparing microwave dielectric ceramic material according to claim 5, characterized in that: in the step (5), the sintering temperature is 1280-1310 ℃ in a carbon rod furnace, and the sintering time is 3 hours.
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