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CN-122010544-A - Low-dielectric silicate LTCC material with stable temperature and preparation method thereof

CN122010544ACN 122010544 ACN122010544 ACN 122010544ACN-122010544-A

Abstract

The application provides a low-dielectric silicate LTCC material with stable temperature and a preparation method thereof, and relates to the technical field of low-dielectric microwave dielectric ceramics. The low-dielectric silicate LTCC material is prepared from a compound with a chemical formula of xNa 2 O-yCaO-zSiO 2 -mCaSnSiO 5 -nB 2 O 3 , wherein x is more than or equal to 0.8 and less than or equal to 1.2,1.8, y is more than or equal to 2.2,2.9, z is more than or equal to 3.3,0.6 and less than or equal to m is more than or equal to 1.5, n is more than or equal to 0.03 and less than or equal to 0.1, and the chemical expression of a main crystal phase is Na 2 Ca 2 Si 3 O 9 . The low-dielectric silicate LTCC material with stable temperature prepared by adopting the method overcomes the defect of poor temperature stability in the synthesis of low-dielectric microwave dielectric ceramics in the prior art, and the prepared low-dielectric silicate LTCC material has the characteristics of low dielectric constant, stable temperature and sintering temperature lower than 950 ℃, has the advantages of simple synthesis process, stable main crystal phase component and low raw material price, and is suitable for millimeter wave communication.

Inventors

  • DU KANG
  • WANG SHENGXIANG
  • YE SHUAN
  • XU YUANLU
  • YAN JIAYING
  • LI LINJIE
  • LI CHENGLONG
  • XIONG ZIYI

Assignees

  • 武汉纺织大学

Dates

Publication Date
20260512
Application Date
20260410

Claims (8)

  1. 1. The low-dielectric silicate LTCC material with stable temperature is characterized in that the low-dielectric silicate LTCC material with stable temperature is prepared by adopting a compound with a chemical formula of xNa 2 O-yCaO-zSiO 2 -mCaSnSiO 5 -nB 2 O 3 , wherein x is more than or equal to 0.8 and less than or equal to 1.2,1.8, y is more than or equal to 2.2,2.9, z is more than or equal to 3.3,0.6 and less than or equal to m is less than or equal to 1.5, n is more than or equal to 0.03 and less than or equal to 0.1, the chemical expression of a main crystal phase of the low-dielectric silicate LTCC material is Na 2 Ca 2 Si 3 O 9 , and a glass phase does not exist in phase components.
  2. 2. The temperature-stable low-mesosilicate LTCC material according to claim 1, wherein the dielectric constant epsilon r of the temperature-stable low-mesosilicate LTCC material is 5.0-8.0, the quality factor qxf is 6200 ghz-14300 ghz, and the resonant frequency temperature coefficient τ f is-2.1 ppm/°c to-14.6 ppm/°c.
  3. 3. A method of preparing a temperature stable low dielectric silicate LTCC material as claimed in claim 1 or 2, comprising the steps of: S1, weighing the raw materials of Na 2 CO 3 、CaO、SiO 2 and B 2 O 3 , and proportioning according to the stoichiometric ratio of xNa 2 O-yCaO-zSiO 2 -nB 2 O 3 , wherein x is more than or equal to 0.8 and less than or equal to 1.2,1.8, y is more than or equal to 2.2,2.9 and z is more than or equal to 3.3,0.03 and n is more than or equal to 0.1, uniformly mixing, performing first wet ball milling treatment, and drying and presintering to obtain presintered ceramic powder; S2, weighing raw materials of CaO, snO 2 and SiO 2 , mixing according to the stoichiometric ratio of CaSnSiO 5 , performing secondary wet ball milling treatment after uniform mixing, and drying and presintering to obtain CaSnSiO 5 presintering ceramic powder; S3, mixing the presintered ceramic powder prepared in the step S1 and the CaSnSiO 5 presintered ceramic powder prepared in the step S2 according to the stoichiometric ratio of xNa 2 O-yCaO-zSiO 2 -mCaSnSiO 5 -nB 2 O 3 , performing a third wet ball milling treatment, drying after ball milling treatment, adding an adhesive for granulating, tabletting, and sintering to obtain the low-dielectric silicate LTCC material.
  4. 4. The method for preparing a low-dielectric silicate LTCC material according to claim 3, wherein in the step S1, the pre-sintering temperature is 700-850 ℃ and the pre-sintering time is 5-10 h.
  5. 5. The method for preparing a low-dielectric silicate LTCC material according to claim 3, wherein in the step S2, the presintering temperature is 1050-1150 ℃ and the presintering time is 5-10 h.
  6. 6. The method for producing low-dielectric silicate LTCC material according to claim 3, wherein in the step S3, the sintering temperature is 800-925 ℃ and the sintering time is 5-10 h.
  7. 7. The method for preparing low-dielectric silicate LTCC material according to claim 3, wherein in the steps S1, S2 and S3, the dispersing agents for the first, second and third wet ball milling treatments are absolute ethyl alcohol, the ball milling medium is zirconium balls, and the ball milling time is 5-10 hours.
  8. 8. A method of preparing a low dielectric silicate LTCC material according to claim 3, wherein in step S3, the binder is PVA or paraffin wax.

Description

Low-dielectric silicate LTCC material with stable temperature and preparation method thereof Technical Field The application relates to the technical field of low-dielectric microwave dielectric ceramics, in particular to a low-dielectric silicate LTCC material with stable temperature and a preparation method thereof. Background The low temperature co-fired ceramic (Low Temperature co-FIRED CERAMICS, LTCC) technology is a novel multilayer substrate preparation technology developed in the middle of the 80 s of the 20 th century. The sintering temperature of the technology is lower (below 950 ℃), and the technology can realize co-sintering with metal conductors such as silver, copper and the like, thereby being beneficial to improving the performance of electronic devices. Meanwhile, the unique multilayer cofiring process can remarkably simplify the preparation process and improve the reliability of components. The low-temperature co-firing technology strongly promotes the rapid development of microwave components to the directions of miniaturization, multifunction, high frequency and high reliability. With the advent of the 5G communications era, the development of 5G technology has put more stringent requirements on LTCC materials for electronic components, and particularly in the upcoming millimeter wave and terahertz communications field, the requirements on LTCC materials with ultra-low dielectric constants are urgent. Currently, commercial LTCC materials mainly include glass-ceramic systems and "glass+ceramic" complex phase systems. The existing LTCC material generally contains a large amount of amorphous glass phase, and the introduction of the glass phase can reduce the sintering temperature of the material to below 950 ℃, but can significantly degrade the microwave dielectric property of the material. Meanwhile, the problem of poor temperature stability of the conventional commercial LTCC material is common, the use requirements of devices such as resonators and dielectric antennas are difficult to meet, and the further development of the LTCC integrated module is greatly restricted. Therefore, there is a need to develop a low dielectric constant silicate LTCC material having excellent temperature stability, no glass phase, and low temperature sintering, and a method for preparing the same, so as to solve the above problems of the prior art. Disclosure of Invention The application aims to provide a preparation method of a low-dielectric-constant silicate LTCC material, the sintering temperature of the low-dielectric-constant silicate LTCC material prepared by the method is lower than 950 o ℃, the low-dielectric-constant silicate LTCC material has a low dielectric constant, a high quality factor and a near-zero resonance frequency temperature coefficient, and the development of the low-dielectric-constant silicate LTCC material widens the selection range of the low-dielectric-constant LTCC material. In order to achieve the aim of the application, the application provides a low-dielectric silicate LTCC material with stable temperature, which is prepared by adopting a compound with a chemical formula of xNa 2O-yCaO-zSiO2-mCaSnSiO5-nB2O3, wherein x is more than or equal to 0.8 and less than or equal to 1.2,1.8, y is more than or equal to 2.2,2.9 and less than or equal to y is more than or equal to 3.3,0.6 and less than or equal to m is less than or equal to 1.5, n is more than or equal to 0.03 and less than or equal to 0.1, the chemical expression of a main crystal phase of the low-dielectric silicate LTCC material with stable temperature is Na 2Ca2Si3O9, and no glass phase exists in phase components. Preferably, the dielectric constant epsilon r of the low-dielectric silicate LTCC material with stable temperature is 5.0-8.0, the quality factor Q multiplied by f is 6200 GHz-14300 GHz, and the resonant frequency temperature coefficient tau f is-2.1 ppm/-14.6 ppm/°. Further, the preparation method of the low-dielectric silicate LTCC material stable in temperature comprises the following steps: S1, weighing the raw materials of Na 2CO3、CaO、SiO2 and B 2O3, mixing according to the stoichiometric ratio of xNa 2O-yCaO-zSiO2-nB2O3 (x is more than or equal to 0.8 and less than or equal to 1.2,1.8 and y is more than or equal to 2.2,2.9 and z is more than or equal to 3.3,0.03 and n is more than or equal to 0.1), uniformly mixing, performing first wet ball milling treatment, and drying and presintering to obtain presintered ceramic powder; S2, weighing raw materials of CaO, snO 2 and SiO 2, mixing according to the stoichiometric ratio of CaSnSiO 5, performing secondary wet ball milling treatment after uniform mixing, and drying and presintering to obtain CaSnSiO 5 presintering ceramic powder; S3, mixing the presintered ceramic powder prepared in the step S1 and the CaSnSiO 5 presintered ceramic powder prepared in the step S2 according to the stoichiometric ratio of xNa 2O-yCaO-zSiO2-mCaSnSiO5-nB2O3, performing a thi