CN113135752A - Production method of high-dielectric low-loss high-frequency microwave composite dielectric substrate - Google Patents
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Abstract
A preparation method of a high-dielectric low-loss high-frequency microwave composite dielectric substrate belongs to the field of microwave electronic component ceramic materials, and comprises the following steps: according to molar ratio CaTiO3、Li0.5Sm0.5TiO3Preparing materials to form CLST porcelain powder; ball milling of porcelain powder; sintering at high temperature; carrying out surface treatment on the porcelain powder by using a silane coupling agent; mixing the ceramic powder subjected to surface treatment with polytetrafluoroethylene emulsion; adding a demulsifier to perform demulsification; standing and filtering to form a composite dough; performing calendaring molding or compression molding; and carrying out hot-pressing sintering on the copper foil coated on the two sides of the molded green body to form the high-dielectric low-loss high-frequency microwave composite dielectric substrate. Solves the problems of low dielectric constant, large loss, large temperature coefficient of resonant frequency and no continuous batch production of the existing microwave dielectric ceramic materialThe problem of capacity. The microwave antenna is widely applied to the field of modern microwave electronic communication such as aerospace electronic equipment circuit boards, satellite communication, Beidou system and the like.
Description
Technical Field
The invention belongs to the field of electronic components, in particular to the field of microwave electronic components, and further belongs to the field of microwave electronic component ceramic materials.
Background
Microwave dielectric ceramics (MWDC) refers to ceramic materials which are used as dielectric materials in microwave frequency band (300 MHz-300 GHz) circuits and can perform one or more functions. In microwave electronic components, microwave dielectric ceramics are used as key materials for manufacturing microwave resonators and filters, and ideal performance of the microwave dielectric ceramics is represented as follows: the volume miniaturization of the device is realized by high dielectric constant, the working high frequency of the device is ensured by high quality factor, and the working stability of the device is ensured by near-zero resonant frequency temperature coefficient. At present, although the widely adopted microwave dielectric ceramic material meets the use requirements of some electronic components in terms of performance, with the continuous and deep research on satellite application, deep space exploration and manned space related, high-quality circuit boards with high capacity, high frequency band, high power and the like become the mainstream development direction of space electronic equipment, the microwave composite dielectric substrate which is the main material used by microwave radio frequency circuits and antennas has the requirements of high dielectric, low loss and good high-frequency stability, and at present, the domestic microwave dielectric material is mainly produced and transformed from the traditional low-frequency copper-clad plate and is concentrated in the direction of impregnating glass fiber cloth with polytetrafluoroethylene emulsion, the dielectric constant of polytetrafluoroethylene resin is about 2.2, the dielectric constant of glass fiber cloth is about 6, even if ceramic filler is introduced to prepare the glass fiber cloth/ceramic/polytetrafluoroethylene three-phase composite dielectric substrate, the dielectric constant of the structure is difficult to be more than 10 under 10Ghz, it is difficult to meet the development requirements of large capacity, miniaturization and high integration. Therefore, the microwave composite dielectric substrate with the dielectric constant of more than 13 and the loss of less than 0.004 at 10GHz is prepared by preparing the microwave ceramic powder with the high dielectric constant, filling polytetrafluoroethylene for compounding, mixing, demulsifying, rolling, hot-pressing, sintering and the like, and the method has continuous batch production capacity.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The purpose of the invention is: the microwave composite dielectric substrate with the dielectric constant of more than 13 and the loss of less than 0.004 under 10GHz is prepared, and has continuous batch production capability. Solves the problems of low dielectric constant, large loss, large temperature coefficient of resonance frequency and no continuous batch production capability of the existing microwave dielectric ceramic material.
The technical conception adopted by the invention is as follows: by preparing the high-dielectric microwave ceramic powder as a filler, low-dielectric glass fiber cloth is not used any more, and pure ceramic is adopted to fill polytetrafluoroethylene, the problem that the traditional production process is difficult to prepare the high-dielectric, low-loss and high-frequency microwave composite dielectric substrate is solved.
Therefore, the invention provides a preparation method of a high-dielectric low-loss high-frequency microwave composite dielectric substrate, as shown in fig. 1 and fig. 2. The method specifically comprises the following steps:
(1) CLST porcelain powder (CaO-Li)2O-Sm2O3-TiO2Ceramic powder is called CLST ceramic powder for short) as raw material: CaCO is added according to a molar ratio of 1:13And Ti02Mixing the raw materials, sintering the mixture for 3 hours in a furnace at 1180 ℃ to synthesize CaTiO3Porcelain powder; mixing Li with a molar ratio of 0.5:0.5:12O、Sm2O3、Ti02Proportioning, sintering at 1120 deg.C for 2 hr to synthesize Li0.5Sm0.5TiO3Porcelain powder;
(2) preparing CLST porcelain powder: adding CaTiO3With Li0.5Sm0.5TiO3Proportioning according to a molar ratio of (0.6-0.8) to (0.4-0.2), sintering for 2-5 h in a high-temperature furnace at 1100-1200 ℃, and synthesizing high-dielectric CLST microwave ceramic powder with a dielectric constant of 120-135 and a frequency temperature coefficient of 60-200 ppm/DEG C;
(3) CLST porcelain powder surface treatment: performing surface treatment on the CLST porcelain powder by using a silane coupling agent;
(4) mixing CLST porcelain powder with emulsion: mixing the CLST ceramic powder subjected to surface treatment according to (1-x) CLST ceramic powder and x polytetrafluoroethylene emulsion, wherein x is the mass percentage; fully stirring the mixed solution at a high speed by adopting a high-speed stirring device to prepare uniformly mixed polytetrafluoroethylene/ceramic composite emulsion;
(5) demulsifying: a flocculating agent is used as a demulsifier, the flocculating agent is one or more of polyethyleneimine PEI, alcohol and diethyl ether, a high-speed stirring device is adopted for full high-speed stirring to separate out a flocculation precipitate of the mixed emulsion, and the whole process is stirred at a high speed;
(6) standing and filtering: fully standing the mixed solution, and filtering to form composite dough;
(7) and (3) pressing and forming: carrying out calendaring molding or compression molding on the composite dough;
(8) hot-pressing and sintering: and carrying out hot-pressing sintering on the copper foil coated on the two sides of the molded green body to form the high-dielectric low-loss high-frequency microwave composite dielectric substrate.
The high-speed stirring device is a high-speed stirrer.
The silane coupling agent is one or two of KH550, Z6214, KH570 and KH 792.
The value range of x is more than or equal to 0.75 and more than or equal to 0.6.
The high-speed stirring speed is 400 r/min-800 r/min, and the high-speed stirring time is 20 min-60 min.
The standing time is 4-10 h.
The high-dielectric low-loss high-frequency microwave composite dielectric substrate prepared by the process has the dielectric constant of more than or equal to 13 under 10Ghz, the loss of less than or equal to 0.004, and the temperature coefficient of the dielectric constant of +/-200 ppm/DEG C, which is a preferred material for preparing a miniaturized and high-integration microwave radio frequency circuit.
The high-dielectric low-loss high-frequency microwave composite dielectric substrate has the following characteristics:
(1) the dielectric constant is more than or equal to 13;
(2) the loss is less than or equal to 0.004.
(3) The frequency can reach 10 Ghz.
(4) The temperature coefficient of dielectric constant is less than +/-200 ppm/DEG C.
(5) Is the preferable material for preparing miniaturized and highly integrated microwave radio frequency circuits.
The high-dielectric low-loss high-frequency microwave composite dielectric substrate is widely applied to the fields of modern microwave electronic communication such as aerospace electronic equipment, mobile communication, electronic countermeasure, satellite communication, a Beidou system (GPS), a Bluetooth technology, a wireless local area network (MLAN) and the Internet of things of high-quality circuit boards with high capacity, high frequency range, high power and the like.
Drawings
FIG. 1 is a schematic diagram of a CLST porcelain powder raw material powder preparation process.
Fig. 2 is a schematic view of a process flow for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate.
Detailed Description
The specific implementation mode of the invention content is as follows:
(1) according to 0.6CaTiO3+0.4Li0.5Sm0.5TiO3Preparing materials according to the molar ratio;
(2) performing planetary ball milling;
(3) sintering at high temperature, wherein the sintering temperature is 1150 ℃ and the time is 2 hours, and preparing high-dielectric microwave porcelain powder for later use;
(4) performing surface treatment on the porcelain powder by using a silane coupling agent KH550, wherein the using amount of the KH550 is 1.5 wt% of the mass of the porcelain powder;
(5) mixing the materials according to (1-x) CLST porcelain powder and x polytetrafluoroethylene emulsion (wherein x is the mass percent, x is more than or equal to 0.7 and more than or equal to 0.6), and fully stirring;
(6) adding alcohol as a demulsifier, and stirring at a high speed of 400 r/min-800 r/min for 30 min;
(7) standing the mixed solution for 6h, and filtering to obtain a composite dough;
(8) rolling and molding the composite dough;
(9) and (4) carrying out hot-pressing sintering on the formed green body coated with copper foil on two sides to form the high-dielectric low-loss high-frequency microwave composite dielectric substrate. The sintering temperature is 375 ℃, the pressure is 8Mpa, and the time is 2 h.
The high-frequency microwave composite dielectric substrates with different components are tested, and the electrical performance parameters are shown in table 1.
Table 1 test table for electrical performance parameters of high-frequency microwave composite dielectric substrate with different components
Finally, it should be noted that: the above examples are merely examples for clarity of illustration, and the present invention includes but is not limited to the above examples, which are not necessarily exhaustive of all embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Embodiments that meet the requirements of the present invention are within the scope of the present invention.
Claims (10)
1. A preparation method of a high-dielectric low-loss high-frequency microwave composite dielectric substrate comprises the following steps:
(1) preparing CLST porcelain powder raw materials: CaCO is added according to a molar ratio of 1:13And Ti02Mixing the raw materials, sintering the mixture for 3 hours in a furnace at 1180 ℃ to synthesize CaTiO3Porcelain powder; mixing Li with a molar ratio of 0.5:0.5:12O、Sm2O3、Ti02Proportioning, sintering at 1120 deg.C for 2 hr to synthesize Li0.5Sm0.5TiO3Porcelain powder;
(2) preparing CLST porcelain powder: adding CaTiO3With Li0.5Sm0.5TiO3Proportioning according to a molar ratio of (0.6-0.8) to (0.4-0.2), sintering for 2-5 h in a high-temperature furnace at 1100-1200 ℃, and synthesizing high-dielectric CLST microwave ceramic powder;
(3) CLST porcelain powder surface treatment: performing surface treatment on the CLST porcelain powder by using a silane coupling agent;
(4) mixing CLST porcelain powder with emulsion: according to the mass percentage, the CLST ceramic powder subjected to surface treatment is prepared according to (1-x) CLST ceramic powder and x polytetrafluoroethylene emulsion, and a high-speed stirring device is adopted to fully stir the mixed solution at high speed so as to prepare uniformly mixed polytetrafluoroethylene/ceramic composite emulsion;
(5) demulsifying: adding a demulsifier, fully stirring at a high speed by adopting a high-speed stirring device to separate out a flocculation precipitate of the mixed emulsion, and stirring at a high speed in the whole process;
(6) standing and filtering: fully standing the mixed solution, and filtering to form composite dough;
(7) and (3) pressing and forming: carrying out calendaring molding or compression molding on the composite dough;
(8) hot-pressing and sintering: and carrying out hot-pressing sintering on the copper foil coated on the two sides of the molded green body to form the high-dielectric low-loss high-frequency microwave composite dielectric substrate.
2. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the high-dielectric CLST microwave ceramic powder has a dielectric constant of 120-135 and a frequency temperature coefficient of 60-200 ppm/DEG C.
3. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the silane coupling agent is one or two of KH550, Z6214, KH570 and KH 792.
4. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the value range of x is more than or equal to 0.75 and more than or equal to 0.6.
5. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the high-speed stirring device is a high-speed stirrer.
6. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the high-speed stirring speed is 400 r/min-800 r/min, and the high-speed stirring time is 20 min-60 min.
7. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the demulsifier is a flocculant.
8. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 7, wherein the method comprises the following steps: the flocculating agent is one or more of polyethyleneimine PEI, alcohol and diethyl ether.
9. The method for preparing a high-dielectric low-loss high-frequency microwave composite dielectric substrate according to claim 1, wherein the method comprises the following steps: the standing time is 4-10 h.
10. The preparation method of the high-dielectric low-loss high-frequency microwave composite dielectric substrate as claimed in claim 1, characterized by comprising the following detailed steps:
(1) according to 0.6CaTiO3+0.4Li0.5Sm0.5TiO3Preparing materials according to the molar ratio;
(2) performing planetary ball milling;
(3) sintering at high temperature, wherein the sintering temperature is 1150 ℃ and the time is 2 hours, and preparing high-dielectric microwave porcelain powder for later use;
(4) performing surface treatment on the porcelain powder by using a silane coupling agent KH550, wherein the using amount of the KH550 is 1.5 wt% of the mass of the porcelain powder;
(5) mixing (1-x) CLST porcelain powder and x polytetrafluoroethylene emulsion, and fully stirring, wherein x is more than or equal to 0.7 and more than or equal to 0.6;
(6) adding a flocculating agent as a demulsifier, and stirring at a high speed of 400 r/min-800 r/min for 30 min;
(7) standing the mixed solution for 6h, and filtering to obtain a composite dough;
(8) rolling and molding the composite dough;
(9) and carrying out hot-pressing sintering on the formed green body coated with copper foil on two sides, wherein the sintering temperature is 375 ℃, the pressure is 8Mpa, and the time is 2 hours, so as to form the high-dielectric low-loss high-frequency microwave composite dielectric substrate.
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Cited By (3)
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| CN113735580A (en) * | 2021-09-01 | 2021-12-03 | 北京工业大学 | Complex-phase microwave dielectric ceramic and cold sintering preparation method thereof |
| CN114751733A (en) * | 2022-04-25 | 2022-07-15 | 中国振华集团云科电子有限公司 | Production method of spherical ceramic filler with low temperature coefficient |
| CN115503306A (en) * | 2022-09-22 | 2022-12-23 | 泰州市旺灵绝缘材料厂 | Ultrathin superfine glass fiber cloth ceramic high-frequency copper foil-clad substrate and manufacturing process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113735580A (en) * | 2021-09-01 | 2021-12-03 | 北京工业大学 | Complex-phase microwave dielectric ceramic and cold sintering preparation method thereof |
| CN113735580B (en) * | 2021-09-01 | 2022-06-24 | 北京工业大学 | Complex-phase microwave dielectric ceramic and cold sintering preparation method thereof |
| CN114751733A (en) * | 2022-04-25 | 2022-07-15 | 中国振华集团云科电子有限公司 | Production method of spherical ceramic filler with low temperature coefficient |
| CN115503306A (en) * | 2022-09-22 | 2022-12-23 | 泰州市旺灵绝缘材料厂 | Ultrathin superfine glass fiber cloth ceramic high-frequency copper foil-clad substrate and manufacturing process |
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