CN113480303B - Aluminate-based low-dielectric microwave dielectric ceramic and preparation method thereof - Google Patents
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Abstract
The invention discloses aluminate-based low-dielectric-constant microwave dielectric ceramic and a preparation method thereof, wherein the main crystal phase of the microwave dielectric ceramic has a garnet crystal structure, and the specific chemical composition is (2 + x) CaO-0.5Ln 2 O 3 ‑(2‑y)ZrO 2 ‑(x+y)MO 2 ‑1.5Al 2 O 3 Ln is Y, la, lu, gd or other lanthanide elements, M is Hf, sn or Ti, x is more than or equal to 0 and less than or equal to 0.5, and Y is more than or equal to 0 and less than or equal to 2.0. The dielectric constant of the microwave dielectric ceramic is 10.81-13.52, the quality factor is 72441 GHz-121930 GHz, and the temperature coefficient of the resonant frequency is +0.50 ppm/DEG C-35.48 ppm/DEG C. In the preparation process, the pre-sintering condition of the ceramic material is that the temperature is kept at 1300 ℃ for 5 hours, and the sintering condition is that the temperature is kept at 1500-1600 ℃ for 10 hours. The microwave dielectric ceramic prepared by the method has the characteristics of low dielectric constant, high quality factor and adjustable and controllable resonant frequency temperature coefficient to be near zero, and is suitable for preparing microwave communication devices such as dielectric substrates, dielectric resonators, dielectric antennas and the like.
Description
Technical Field
The invention belongs to the technical field of microwave dielectric ceramics, and particularly relates to an aluminate-based low-dielectric microwave dielectric ceramic and a preparation method thereof.
Background
The microwave dielectric ceramic is a basic material for preparing passive devices such as high-frequency capacitors, dielectric substrates, dielectric waveguide filters, dielectric antennas and the like, and is widely applied to various wireless communication systems. With the gradual commercial phase of 5G communication, the integration level and the working frequency of communication equipment are continuously improved, and the problems of signal time delay, signal crosstalk, system heating and the like are increasingly highlighted. The low dielectric constant and low dielectric loss microwave dielectric ceramic can effectively improve the transmission rate of microwave signals, reduce the signal energy loss and meet the requirements of 5G and other microwave millimeter wave communication, thereby gradually becoming the focus of attention of academia and industry and developing novel low dielectric microwave dielectric ceramic to be right at the time.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an aluminate-based low-dielectric microwave dielectric ceramic and a preparation method thereof, so that the problems of high signal delay, high energy loss, high system heating and the like in the microwave communication technology are solved.
In order to achieve the purpose, the invention provides an aluminate-based low-dielectric microwave dielectric ceramic and a preparation method thereof, wherein the chemical formula of the main crystal phase of the ceramic is (2 +)x)CaO-0.5Ln 2 O 3 -(2-y)ZrO 2 -(x+y)MO 2 -1.5Al 2 O 3 In whichLnIs Y, la, lu, gd or other lanthanide elements,Mhf, sn or Ti is more than or equal to 0x≤0.5，0≤y≤2.0。
Furthermore, the dielectric constant of the microwave dielectric ceramic is 10.81 to 13.52.
Furthermore, the quality factor of the microwave dielectric ceramic is 72441 GHz-121930 GHz.
Furthermore, the resonant frequency temperature coefficient of the microwave dielectric ceramic is +0.50 ppm/DEG C to-35.48 ppm/DEG C.
The invention provides a preparation method of aluminate-based low-dielectric microwave dielectric ceramic, which comprises the following steps:
(1) Mixing CaCO 3 、Ln 2 O 3 、ZrO 2 、MO 2 And Al 2 O 3 According to chemical formula (2 +x)CaO-0.5Ln 2 O 3 -(2-y)ZrO 2 -(x+y)MO 2 -1.5Al 2 O 3 The materials are mixed to obtain a mixed raw material, wherein,Lnis Y, la, lu, gd or other lanthanide elements,Mhf, sn or Ti is more than or equal to 0x≤0.5，0≤yBall-milling, drying and sieving the mixed raw materials in sequence to obtain powder with uniform particles, wherein the particle size of the powder is less than or equal to 2.0;
(2) Presintering the powder material at 1300 ℃ for 5 hours to obtain presintering powder material, sequentially performing ball milling, drying and sieving on the presintering powder material to obtain presintering ceramic powder, granulating the presintering ceramic powder material by using a binder, performing pressure molding to obtain a ceramic blank, and sintering the ceramic blank at 1500-1600 ℃ for 10 hours to obtain the microwave dielectric ceramic.
Further, the specific implementation manner of the ball milling is as follows:
adding the mixed raw materials and absolute ethyl alcohol into a polyester ball milling tank filled with zirconium balls, and carrying out ball milling for 16 hours in a planetary ball mill.
Further, the specific implementation manner of drying is as follows:
and (3) drying the mixed raw materials subjected to ball milling in a forced air drying oven at 90 ℃ for 24 hours.
In general, compared with the prior art, the above technical solutions conceived by the present invention can achieve the following beneficial effects:
(1) The dielectric constant of the aluminate-based low-dielectric microwave dielectric ceramic prepared by the invention is 10.81 to 13.52, the transmission rate of microwave signals in the medium can be improved, and the problem of signal time delay is relieved.
(2) The aluminate-based low-dielectric microwave dielectric ceramic prepared by the invention not only has low dielectric constant, but also has high quality factor, and the temperature coefficient of the resonant frequency can be regulated to be close to zero. Therefore, the microwave dielectric ceramic prepared by the invention has good performance and can be used in microwave communication devices such as dielectric waveguide filters, dielectric resonators, dielectric antennas and the like.
(3) The preparation steps of the invention are ball milling, drying and sieving in sequence, which aims to mix the raw materials evenly, refine the powder particles and obtain the microwave dielectric ceramic with better quality after sintering at moderate temperature.
Drawings
FIG. 1 is a flow chart of a method for preparing an aluminate-based low dielectric microwave dielectric ceramic according to an embodiment of the present invention.
FIG. 2 is an X-ray diffraction pattern of an aluminate-based low dielectric microwave dielectric ceramic sample provided by an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, a method for preparing an aluminate-based low dielectric microwave dielectric ceramic comprises:
(1) CaCO with purity of more than 99.5 percent 3 、Ln 2 O 3 、ZrO 2 、MO 2 And Al 2 O 3 According to chemical formula (2 +x)CaO-0.5Ln 2 O 3 -(2-y)ZrO 2 -(x+y)MO 2 -1.5Al 2 O 3 The ingredients are mixed to obtain a mixed raw material, wherein,Lny, la, lu, gd or other lanthanides,Mhf, sn or Ti is more than or equal to 0x≤0.5，0≤yBall-milling, drying and sieving the mixed raw materials in sequence to obtain powder with uniform particles, wherein the particle size of the powder is less than or equal to 2.0;
(2) Presintering the uniformly mixed raw materials in the step (1) at 1300 ℃ for 5 hours to obtain presintering powder, sequentially performing ball milling, drying and sieving on the presintering powder to obtain presintering ceramic powder, granulating the presintering ceramic powder by using a binder, then performing pressure forming to obtain a ceramic blank, and sintering the ceramic blank at 1500-1600 ℃ for 10 hours to obtain the microwave dielectric ceramic.
The preferred embodiment of the invention has the following specific implementation modes of ball milling, drying and sieving:
according to the following steps: 1.6, respectively adding the mixed raw materials and absolute ethyl alcohol into a polyester ball milling tank filled with zirconium balls, and carrying out ball milling for 16 hours in a planetary ball mill. And (3) drying the mixed raw materials subjected to ball milling in a forced air drying oven at 90 ℃ for 24 hours. And (4) sieving the dried mixed raw materials by a 40-mesh sieve.
In the embodiment of the invention, preferably, the binder is a PVA aqueous solution with the mass fraction of 5%, the addition amount of the binder is 8wt% of the mass of the powder, the pressure during pressure molding is 150MPa, the diameter of the ceramic blank is 12mm, and the height of the ceramic blank is 6mm.
Table 1 shows the formulations of the present invention prepared in examples 1-11 and the performance parameters of the prepared aluminate-based low dielectric microwave dielectric ceramics.
TABLE 1 microwave dielectric Properties of examples 1-11
To test the microwave dielectric properties of the microwave dielectric ceramics prepared in examples 1-11, the microwave dielectric ceramics prepared in examples 1-11 were first ground on a 600 mesh diamond table, then ultrasonically cleaned in deionized water, and finally dried in a 90 ℃ forced air drying oven for 24 hours. And (3) analyzing the dielectric property of the sample by adopting a parallel plate resonant cavity method, wherein the test frequency is 9 GHz-12 GHz. The resonance frequency temperature coefficient of the sample is obtained by measuring the change rate of the resonance frequency of the parallel plate resonator along with the temperature, and the measurement temperature range is 30-80 ℃. It can be seen that the dielectric constant of the microwave dielectric ceramic prepared by the embodiment of the invention is 10.81 to 13.52, the quality factor is 72441GHz to 121930GHz, and the temperature coefficient of the resonance frequency is +0.50 ppm/DEG C to-35.48 ppm/DEG C.
In thatLn=Y，MIn the case of = Tix=0.19, yAnd =0.3, the microwave dielectric ceramic prepared in embodiment 7 of the present invention satisfies the use requirements of low dielectric constant, high quality factor, and near-zero temperature coefficient of resonance frequency, and can be used for preparing electronic components such as high-frequency capacitors, dielectric waveguide filters, dielectric resonators, and dielectric antennas.
It will be understood by those skilled in the art that the foregoing is only an exemplary embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.
Claims (2)
1. An aluminate-based low dielectric microwave dielectric ceramic, comprising: the chemical formula of the main crystal phase of the ceramic is (2 +x)CaO-0.5Ln 2 O 3 -(2-y)ZrO 2 -(x+y)MO 2 -1.5Al 2 O 3 In whichLnIs Y, la, lu or Gd element,Mhf, sn or Ti is more than or equal to 0x≤0.5，0≤yLess than or equal to 2.0; the ceramic has a dielectric constant of 10.81 to 13.52, a quality factor of 72441GHz to 121930GHz, and a temperature coefficient of resonance frequency of +0.50 ppm/DEG C to-35.48 ppm/DEG C.
2. The method of claim 1, wherein the aluminate-based low dielectric microwave dielectric ceramic comprises the following steps:
(1) Mixing CaCO 3 、Ln 2 O 3 、ZrO 2 、MO 2 And Al 2 O 3 Weighing the ingredients according to the chemical formula in claim 1, and then pouring the weighed raw materials into a ball milling tank in sequence to obtain mixed raw materials;
(2) Adding absolute ethyl alcohol with the mass of 1.6 times of that of the powder into a ball milling tank, ball milling for 16 hours on a planetary ball mill at the rotating speed of 360r/min, placing the ball-milled slurry in a 90 ℃ oven for 24 hours, and sieving the powder through a 40-mesh nylon sieve after the powder is completely dried;
(3) Pouring the sieved powder into a corundum crucible, and presintering for 5 hours in a high-temperature furnace at 1300 ℃ to obtain presintered powder;
(4) Ball-milling, drying and sieving the pre-sintered powder again according to the steps, then adding 8wt% of binder to granulate the powder, and finally applying 150MPa pressure to perform compression molding to obtain a ceramic blank;
(5) Sintering the ceramic blank at 1500-1600 ℃ for 10 hours to obtain the microwave dielectric ceramic.
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