Search

CN-118084466-B - Rare earth oxide doped modified zinc silicate ceramic for microwave device and preparation method thereof

CN118084466BCN 118084466 BCN118084466 BCN 118084466BCN-118084466-B

Abstract

The invention provides rare earth oxide doped modified zinc silicate ceramic for a microwave device and a preparation method thereof, relates to the field of information function ceramic materials, and can be widely applied to the fields of microwave adjustable devices, particularly filters and the like. The ceramic material comprises a main material Zn 2‑ x SiO 4‑x and a modified additive RO rare earth oxide (RO is selected from Zn 2‑x‑y R y SiO 4‑x consisting of La 2 O 3 ,CeO 2 ,Pr 6 O 11 ,Nd 2 O 3 ,Sm 2 O 3 ,Eu 2 O 3 ,Gd 2 O 3 ,Dy 2 O 3 ,Ho 2 O 3 ,Er 2 O 3 ,Tm 2 O 3 ,Yb 2 O 3 ,Lu 2 O 3 ）, wherein x is more than or equal to 0 and less than or equal to 0.4, y is more than or equal to 0 and less than or equal to 2. The steps are as follows, znO, siO 2 and RO are mixed according to a certain proportion, and the mixture is subjected to ball milling, drying, sieving, presintering, secondary ball milling, granulating, sieving, blank making and sintering to obtain the zinc silicate-based microwave dielectric ceramic.

Inventors

  • WEN WEI
  • JIANG TING
  • YANG WEIZE
  • MA XINGYUN
  • LU YAOFU

Assignees

  • 西华师范大学

Dates

Publication Date
20260505
Application Date
20240306

Claims (7)

  1. 1. The rare earth oxide doped modified zinc silicate ceramic for the microwave device comprises a main material and a modified additive, and is characterized in that the main material Zn 2-x SiO 4-x and the modified additive RO rare earth oxide form Zn 2-x-y R y SiO 4-x , wherein x is more than or equal to 0 and less than or equal to 0.4, y is more than or equal to 0.2, and RO is selected from La 2 O 3 ,Pr 6 O 11 ,Nd 2 O 3 ,Sm 2 O 3 ,Eu 2 O 3 ,Gd 2 O 3 ,Dy 2 O 3 ,Ho 2 O 3 ,Er 2 O 3 ,Tm 2 O 3 ,Yb 2 O 3 ,Lu 2 O 3 ; the preparation method of the rare earth oxide doped modified zinc silicate ceramic comprises the following steps: S1, proportioning ZnO, RO and SiO 2 according to the stoichiometric ratio of a chemical formula Zn 2-x-y R y SiO 4-x , wherein x is more than or equal to 0 and less than or equal to 0.4, and y is more than or equal to 0.2; S2, mixing materials, namely performing wet ball milling on the prepared ZnO, RO and SiO 2 to obtain slurry; s3, drying, namely drying the slurry to constant weight to obtain a dried mixture; S4, presintering, namely dispersing the mixture, presintering for the first time to synthesize Zn 2-x-y R y SiO 4-x compound powder, wherein the presintering temperature is 1000-1200 ℃, the temperature rising rate from room temperature to presintering treatment is 1-10 ℃ per minute, the heat preservation time is 2-6 hours, and the temperature is reduced to 600 ℃ at 2-10 ℃ per minute, and then the temperature is reduced to room temperature along with a furnace; S5 ball milling, namely performing wet secondary ball milling on the presintered synthesized Zn 2-x-y R y SiO 4-x compound powder to form Zn 2-x-y R y SiO 4-x compound slurry; S6, drying, namely drying the Zn 2-x-y R y SiO 4-x compound slurry to constant weight to obtain Zn 2-x-y R y SiO 4-x compound powder; S7, granulating and pressing, namely sieving the dried Zn 2-x-y R y SiO 4-x compound powder, adding an adhesive, uniformly mixing, sieving, and pressing to obtain a ceramic green body; And S8, glue discharging and sintering, namely heating the ceramic green body to a glue discharging temperature, preserving heat to remove an adhesive, then heating to a high temperature for sintering, then cooling to a temperature below 300 ℃ and then cooling with a furnace, wherein the glue discharging temperature in the step S8 is 500-700 ℃, the glue discharging time is 1-3 h, the sintering temperature is 1200-1325 ℃, the heating rate is 1-10 ℃ per minute, the heat is preserved for 2-8 hours, and cooling to the room temperature with the furnace after cooling to 300 ℃ at 1-10 ℃ per minute.
  2. 2. The rare earth oxide doped modified zinc silicate ceramic for microwave devices according to claim 1, wherein the ZnO, RO, siO 2 in step S1 has a purity of 99.0% -99.99%.
  3. 3. The rare earth oxide doped modified zinc silicate ceramic for the microwave device according to claim 1, wherein the wet ball milling in the steps S2 and S5 adopts a polytetrafluoroethylene ball milling tank, zirconia balls and a planetary ball mill, wherein the ball milling auxiliary agent is deionized water, the volume ratio of powder to zirconia balls to deionized water is=1:3-7:8-12, the rotational speed of the ball mill is 200-400 r/min, and the ball milling time is 6-24 h.
  4. 4. The rare earth oxide doped modified zinc silicate ceramic for microwave devices according to claim 1, wherein the slurry drying temperature in the steps S3 and S6 is 80-150 ℃ for 12-24 hours.
  5. 5. A rare earth oxide doped modified zinc silicate ceramic for use in a microwave device according to claim 1, wherein said steps S4, S5, S6 are jointly performed as optional steps, i.e. steps S1-S8 are jointly performed, or steps S1, S2, S3, S7, S8 are jointly performed.
  6. 6. The rare earth oxide doped modified zinc silicate ceramic for microwave devices according to claim 1, wherein the binder in the step S7 is 5-10wt% polyvinyl alcohol, a 40-200 mesh standard sieve is adopted, the pressure of powder pressing is 100-300 mpa, and the pressure maintaining time is 10-120 seconds.
  7. 7. Use of a rare earth oxide doped modified zinc silicate ceramic according to any of claims 1 to 6 for the manufacture of a microwave device comprising a stacked antenna, a dielectric antenna, a filter and a resonator.

Description

Rare earth oxide doped modified zinc silicate ceramic for microwave device and preparation method thereof Technical Field The invention belongs to the technical field of wireless communication and electronic ceramic materials, and particularly relates to rare earth oxide doped modified zinc silicate ceramic for a microwave device and a preparation method thereof. Background The discovery and development of electromagnetic waves greatly promote the progress of human society, and the electromagnetic waves in the microwave frequency range are more closely related to people and things. The development of mobile communication technology is rapid, new generation of mobile communication technology can be generated every ten years, the frequency of electromagnetic wave used by each generation of mobile communication technology reaches a new height, and electromagnetic wave with high frequency can carry a large amount of information, but has the defects of poor barrier bypassing capability, easy attenuation and the like, and can easily cause frame loss of signals in the transmission process. In order to meet the development requirements of 5G/6G communication technology, dielectric ceramics with low dielectric constant, high quality factor and near zero resonance frequency temperature have been attracting attention in recent years as key materials for components such as dielectric resonators, dielectric filters, antennas, substrates and the like. The low dielectric constant improves the transmission efficiency of the electric signal, and the high quality factor ensures the frequency selectivity in the signal transmission process. The Zn 2-xSiO4-x dielectric material has excellent dielectric property, low dielectric constant epsilon r (6.5), high quality factor Q multiplied by f (198400 GHz) and relatively negative resonant frequency temperature coefficient tau f (-41.6 ppm/°C). Although the dielectric constant and the quality factor of the material are excellent, the adopted preparation method is complex, when the material is prepared by adopting a conventional solid phase reaction method, the volatilization of ZnO exists at high temperature, a second phase of ZnO can be generated due to a narrow sintering interval, and the problems of more pores of a sintered sample and the like increase the dielectric loss, so that the quality factor is seriously reduced. In order to solve the technical problems, the rare earth oxide doped modified zinc silicate ceramic for the microwave device and the preparation method thereof are provided. Disclosure of Invention Example embodiments will now be described more fully. However, the exemplary embodiments can be embodied in many different forms and should not be construed as limited to the examples set forth herein, but rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the exemplary embodiments to those skilled in the art. Furthermore, the described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a thorough understanding of embodiments of the application. One skilled in the relevant art will recognize, however, that the application may be practiced without one or more of the specific details, or with other methods, components, devices, steps, etc. In other instances, well-known methods, devices, implementations, or operations are not shown or described in detail to avoid obscuring aspects of the application. Unless otherwise indicated, the various raw materials, reagents, instruments and equipment, and the like, used in the present application are commercially available or may be prepared by existing methods. In view of the above-mentioned circumstances in the prior art, the present invention aims to provide a rare earth oxide doped modified zinc silicate ceramic for microwave devices and a preparation method thereof, so as to solve the problems of high sintering temperature and narrow sintering interval of Zn 2-xSiO4-x ceramic, and deteriorated dielectric properties. The above object of the present invention is achieved by the following means. A rare earth oxide doped modified zinc silicate ceramic for microwave devices and a preparation method thereof are characterized by comprising the following steps: (1) The ingredients are ZnO, RO and SiO 2 according to the stoichiometric ratio of the chemical formula Zn 2-x-yRySiO4-x (RO is selected from La2O3,CeO2,Pr6O11,Nd2O3,Sm2O3,Eu2O3,Gd2O3,Dy2O3,Ho2O3,Er2O3,Tm2O3,Yb2O3,Lu2O3）,, wherein x=0.2, 0≤y≤2, the gradient is 0.05, and particularly preferably y=0.2; (2) Mixing, namely performing wet ball milling on the prepared ZnO, RO and SiO 2 to obtain slurry, wherein the wet ball milling can be performed by adopting a polytetrafluoroethylene ball milling tank, zirconia balls and a planetary ball mill, wherein the ball milling aux