CN113563052A - Borate-based low-dielectric microwave dielectric ceramic and preparation method thereof - Google Patents
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Abstract
The invention discloses borate-based low-dielectric-constant microwave dielectric ceramic and a preparation method thereof, wherein the chemical composition of the microwave dielectric ceramic is CaxB2O3+xWherein x is more than or equal to 0.3 and less than or equal to 3.0. The dielectric constant of the microwave dielectric ceramic is 5.62 to 10.12, the quality factor is 13161GHz to 52416GHz, and the temperature coefficient of the resonant frequency is-20.42 ppm/DEG C to-5465 ppm/. degree.C. The ceramic material is heated to 700 ℃ at the speed of 5 ℃/min and is insulated for 3 hours to complete the presintering synthesis, and is heated to 750-1275 ℃ at the speed of 5 ℃/min and is insulated for 3 hours to complete the sintering. The microwave dielectric ceramic prepared by the invention has low dielectric constant, high quality factor and lower sintering temperature, and is suitable for preparing microwave communication devices such as LTCC substrates, dielectric resonators, filters, dielectric antennas and the like.
Description
Technical Field
The invention belongs to the technical field of microwave dielectric ceramics, and particularly relates to borate-based low-dielectric microwave dielectric ceramics and a preparation method thereof.
Background
The microwave dielectric ceramic is a key material for preparing electronic components such as radio frequency capacitors, circuit substrates, dielectric filters, dielectric antennas and the like, so that the microwave dielectric ceramic is widely applied to various wireless communication systems. With the gradual expansion of communication frequency spectrum to high frequency range, the microwave millimeter wave communication is gradually popularized, which makes the integration level and working frequency of communication equipment continuously improved, thereby causing the problems of signal delay, signal crosstalk, system heating and the like to be more and more severe. Electronic components prepared by using low dielectric microwave dielectric ceramics as a base material can effectively alleviate the problems and meet the requirements of microwave and millimeter wave communication represented by 5G communication, so that the development of novel low dielectric microwave dielectric ceramics is urgent.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides borate-based low-dielectric microwave dielectric ceramic and a preparation method thereof, so that the problems of signal delay, signal crosstalk, system heating and the like in the prior art are solved.
In order to achieve the purpose, the invention provides borate-based low-dielectric microwave dielectric ceramic and a preparation method thereof, wherein the chemical formula of the main crystal phase of the ceramic is CaxB2O3+xWherein x is more than or equal to 0.3 and less than or equal to 3.0.
Furthermore, the dielectric constant of the microwave dielectric ceramic is 5.62-10.12.
Furthermore, the quality factor of the microwave dielectric ceramic is 13161 GHz-52416 GHz.
Furthermore, the resonant frequency temperature coefficient of the microwave dielectric ceramic is-20.42 ppm/DEG C to-54.65 ppm/DEG C.
The invention provides a preparation method of borate-based low-dielectric microwave dielectric ceramic, which comprises the following steps:
(1) mixing CaCO3And H3BO3According to the chemical formula CaxB2O3+xMixing, wherein x is more than or equal to 0.3 and less than or equal to 3.0, and weighing H to compensate boron element volatilized at high temperature3BO3When the powder is excessive by 15 wt%, ball milling, drying and sieving are carried out on the mixed raw materials in sequence to obtain powder with uniform particles;
(2) presintering the powder in the step (1) at 700 ℃ for 3 hours, sequentially carrying out ball milling, drying and sieving on the presintered powder to obtain presintered ceramic powder, granulating the presintered ceramic powder by using a binder, then carrying out pressure forming to obtain a ceramic blank, and sintering the ceramic blank at 750-1275 ℃ for 3 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 12 hours in a planetary ball mill.
Further, the specific implementation manner of the burn-in is as follows:
putting the powder into a corundum crucible, then placing the corundum crucible into a high-temperature furnace, heating the corundum crucible to 700 ℃ at the speed of 5 ℃/min, then preserving the heat for 3 hours, and then cooling the corundum crucible to room temperature along with the furnace.
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 12 h.
Further, the specific implementation manner of sintering is as follows:
placing the ceramic blank on a backing plate, then placing the ceramic blank in a high-temperature furnace, heating to 550 ℃ at the speed of 5 ℃/min, then preserving heat for 1 hour to finish glue discharging, then continuously heating to 750-1275 ℃ at the speed of 5 ℃/min, preserving heat for 3 hours, and cooling to room temperature along with the furnace after sintering is finished.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the dielectric constant of the prepared borate-based low-dielectric microwave dielectric ceramic is 5.62-10.12, the transmission rate of microwave signals in the dielectric can be improved, and the problem of signal delay in high-frequency communication is solved.
(2) The borate-based low-dielectric microwave dielectric ceramic prepared by the invention not only has low dielectric constant, but also has high quality factor, and meanwhile, the sintering temperature is lower. The microwave dielectric ceramic prepared by the invention has good performance, and can be used for manufacturing LTCC substrates, filters, dielectric resonators, dielectric antennas and the like.
(3) The preparation steps of the invention are ball milling, drying and sieving in sequence, which are used for uniformly mixing the raw materials and refining powder particles, wherein 15 wt% of H is used for proportioning3BO3The excessive boron element can effectively compensate the volatilization of the boron element during pre-sintering and sintering, and the components are prevented from seriously deviating from the stoichiometric ratio.
Drawings
FIG. 1 is a flow chart of a method for preparing a borate-based low dielectric microwave dielectric ceramic according to an embodiment of the present invention.
FIG. 2 is an X-ray diffraction pattern of a sample of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described below with reference to the following embodiments and the accompanying drawings. The particular embodiments disclosed herein are illustrative only and are not limiting to the invention, as numerous other modifications may be devised by those skilled in the art that will fall within the principles of this disclosure.
As shown in fig. 1, a method for preparing a borate-based low dielectric microwave dielectric ceramic comprises:
(1) mixing CaCO3And H3BO3According to the chemical formula CaxB2O3+xMixing, wherein x is more than or equal to 0.3 and less than or equal to 3.0, and weighing H to compensate boron element volatilized at high temperature3BO3When the mass of the powder is excessive by 15 wt%, the mixed raw materials are sequentially subjected to ball milling, drying and sieving to obtain uniformly mixed powderFeeding;
(2) heating the mixed raw materials in the step (1) to 700 ℃ at a speed of 5 ℃/min, preserving heat for 3 hours to finish pre-sintering, sequentially carrying out ball milling, drying and sieving on the pre-sintered powder to obtain pre-sintered ceramic powder, adding a binder accounting for 8 wt% of the powder mass to granulate the pre-sintered ceramic powder, and finally carrying out pressure molding on the powder to obtain a ceramic blank;
(3) and placing the ceramic blank on a backing plate, then placing the ceramic blank in a high-temperature furnace, heating to 550 ℃ at the speed of 5 ℃/min, preserving heat for 1 hour to finish glue discharging, then continuously heating to 750-1275 ℃ at the speed of 5 ℃/min, preserving heat for 3 hours to finish sintering, and obtaining the microwave dielectric ceramic.
The preferred embodiment of the invention has the following specific implementation modes of ball milling, drying, sieving and sintering:
according to the following steps of 1: 1.5, 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 12 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 12 hours. And (4) sieving the dried mixed raw materials by a 40-mesh sieve. Heating the sieved mixed raw materials to 700 ℃ at the speed of 5 ℃/min, preserving heat for 3 hours to finish pre-sintering, ball-milling again, drying, sieving and granulating, wherein the binder is a PVA aqueous solution with the mass fraction of 5%, the addition amount of the binder is 8 wt% 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 6 mm. And placing the ceramic blank on a backing plate, then placing the ceramic blank in a high-temperature furnace, heating to 550 ℃ at a speed of 5 ℃/min, preserving heat for 1 hour to finish glue discharging, then continuously heating to 750-1275 ℃ at a speed of 5 ℃/min, preserving heat for 3 hours to finish sintering, and obtaining the microwave dielectric ceramic.
Table 1 shows the recipes for preparing examples 1-10 of the present invention and the performance parameters of the prepared borate-based low dielectric microwave dielectric ceramics.
TABLE 1 sintering temperature and microwave dielectric Properties of examples 1-10
To test the microwave dielectric properties of the microwave dielectric ceramics prepared in examples 1-10, the microwave dielectric ceramics prepared in examples 1-10 were first ground on a 1000 mesh diamond table, then ultrasonically cleaned in deionized water, and finally dried in a forced air drying oven at 90 ℃ 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 12 GHz-14 GHz. The temperature coefficient of the resonant frequency of the sample is obtained by measuring the change rate of the resonant 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 5.62-10.12, the quality factor is 13161 GHz-52416 GHz, and the temperature coefficient of the resonance frequency is-20.42 ppm/DEG C to-54.65 ppm/DEG C.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A borate-based low-dielectric microwave dielectric ceramic is characterized in that the chemical formula of the main crystal phase of the ceramic is CaxB2O3+xWherein x is more than or equal to 0.3 and less than or equal to 3.0.
2. The borate-based low dielectric microwave dielectric ceramic of claim 1, wherein the dielectric constant of the microwave dielectric ceramic is 5.62-10.12.
3. The borate-based low dielectric microwave dielectric ceramic as claimed in claim 2, wherein the dielectric constant of the microwave dielectric ceramic is preferably 6.42-8.68.
4. The borate based low dielectric microwave dielectric ceramic of claim 1 or 2, wherein the microwave dielectric ceramic has a quality factor of 13161 GHz-52416 GHz.
5. The borate based low dielectric microwave dielectric ceramic of claim 4, wherein the microwave dielectric ceramic has a quality factor of preferably 34682 GHz-52416 GHz.
6. The borate based low dielectric microwave dielectric ceramic as claimed in claim 1 or 2, wherein the microwave dielectric ceramic has a temperature coefficient of resonant frequency of-20.42 ppm/° c to-54.65 ppm/° c.
7. The borate based low dielectric microwave dielectric ceramic as claimed in claim 6, wherein the resonant frequency temperature coefficient of the microwave dielectric ceramic is preferably-22.62 ppm/° C to-34.17 ppm/° C.
8. The method of any one of claims 1 to 7, comprising:
(1) with CaCO3And H3BO3Is prepared from raw material according to the chemical formula of CaxB2O3+xMixing, wherein x is more than or equal to 0.3 and less than or equal to 3.0, and weighing H to compensate boron element volatilized at high temperature3BO3When the weight of the raw materials is excessive by 15 wt%, the weighed raw materials are poured into a ball milling tank in sequence to obtain mixed raw materials;
(2) adding absolute ethyl alcohol with the mass 1.5 times of that of the powder into a ball milling tank as a ball milling medium, ball milling for 12 hours on a planetary ball mill at the rotating speed of 360r/min, placing the ball-milled slurry in a 90 ℃ oven for 12 hours, and sieving the powder through a 40-mesh nylon sieve after the powder is completely dried;
(3) pouring the powder obtained by the treatment in the steps (1) and (2) into a corundum crucible, and presintering the corundum crucible in a high-temperature furnace at 700 ℃ for 3 hours to obtain presintered powder;
(4) performing ball milling, drying and sieving on the pre-sintered powder again as described in (2), then adding 8 wt% of a binder to granulate the powder, sieving the powder by a 40-mesh sieve, and performing pressure molding to obtain a ceramic blank;
(5) and placing the ceramic blank in a high-temperature furnace, heating to 550 ℃ at the speed of 5 ℃/min, discharging glue for 1 hour, and then continuously heating to 750-1275 ℃ at the speed of 5 ℃/min, and sintering for 3 hours to obtain the microwave dielectric ceramic.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180939A (en) * | 2021-12-28 | 2022-03-15 | 南京工程学院 | Low-dielectric and low-loss boride LTCC material and preparation method thereof |
| CN114702303A (en) * | 2022-03-31 | 2022-07-05 | 电子科技大学 | Microwave dielectric material Ca3B2O6And method for preparing the same |
| CN114988860A (en) * | 2022-06-07 | 2022-09-02 | 华中科技大学温州先进制造技术研究院 | Low-temperature sintered microwave dielectric ceramic and preparation method thereof |
| CN116199498A (en) * | 2023-02-28 | 2023-06-02 | 齐鲁工业大学(山东省科学院) | Low-dielectric-constant borate microwave dielectric ceramic and cold sintering preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114180939A (en) * | 2021-12-28 | 2022-03-15 | 南京工程学院 | Low-dielectric and low-loss boride LTCC material and preparation method thereof |
| CN114702303A (en) * | 2022-03-31 | 2022-07-05 | 电子科技大学 | Microwave dielectric material Ca3B2O6And method for preparing the same |
| CN114988860A (en) * | 2022-06-07 | 2022-09-02 | 华中科技大学温州先进制造技术研究院 | Low-temperature sintered microwave dielectric ceramic and preparation method thereof |
| CN116199498A (en) * | 2023-02-28 | 2023-06-02 | 齐鲁工业大学(山东省科学院) | Low-dielectric-constant borate microwave dielectric ceramic and cold sintering preparation method thereof |
| CN116199498B (en) * | 2023-02-28 | 2023-10-20 | 齐鲁工业大学(山东省科学院) | Low-dielectric-constant borate microwave dielectric ceramic and cold sintering preparation method thereof |
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Application publication date: 20211029 |