CPC C04B 35/495 (2013.01) [C04B 35/462 (2013.01); C04B 35/6262 (2013.01); C04B 35/62655 (2013.01); C04B 35/62695 (2013.01); C04B 35/63416 (2013.01); C04B 35/638 (2013.01); C04B 35/64 (2013.01); H01B 3/12 (2013.01); C04B 2235/3232 (2013.01); C04B 2235/3244 (2013.01); C04B 2235/3255 (2013.01); C04B 2235/3258 (2013.01); C04B 2235/3284 (2013.01); C04B 2235/604 (2013.01); C04B 2235/6562 (2013.01); C04B 2235/6567 (2013.01); C04B 2235/661 (2013.01)] | 3 Claims |
1. A preparation method of an ion-modified microwave dielectric ceramic, comprising the following steps:
preparing a raw material powder, comprising: mixing powders of zinc oxide (ZnO), titanium dioxide (TiO2), niobium oxide (Nb2O5), tungsten oxide (WO3), and zirconium dioxide (ZrO2) according to a chemical formula of Zn0.15Nb0.3[Ti1-x(W1/3Zr1/2)x]0.55O2 to obtain the raw material powder, wherein x is in a range of 0.01 to 0.03; and wherein the ZnO is 12.58-12.67 parts by weight, the TiO2 is 41.11-41.39 parts by weight, the Nb2O5 is 43.93-45.14 parts by weight, the WO3 is 0.44-1.31 parts by weight, and the ZrO2 is 0.35-1.05 parts by weight;
first ball milling, comprising: loading the raw material powder into a ball milling tank, using zirconium balls and deionized water as grinding media of a first planet ball milling and performing the first planet ball milling for 4-6 hours (h) according to a mass ratio of the raw material powder: the zirconium balls: the deionized water of 1: 4-6: 2-4 to obtain a mixed slurry, drying the mixed slurry in an oven after the first planet ball milling and then sieving with a 80-100 mesh sieve to obtain a sieved powder; and sintering the sieved powder in an atmosphere of 900° C.-1,000° C. for 3-5 hours to obtain a pre-sintering material;
second ball milling, comprising: performing a second planet ball milling on the pre-sintering material, zirconium balls, and deionized water for 6-8 hours according to a mass ratio of the pre-sintering material: the zirconium balls: the deionized water of 1: 5-7: 3-5 to obtain a ball-milled material, drying the ball-milled material and then adding a polyvinyl alcohol solution, as a binder, into the ball-milled material, and performing granulation on the ball-milled material added with the polyvinyl alcohol solution to obtain a ceramic raw material; and
compression molding, comprising: performing compression molding operation on the ceramic raw material to obtain a molded ceramic, then performing glue-discharging operation on the molded ceramic at a temperature of 600° C.-650° C. for 2-4 hours with a heating rate of 2-4 degrees Celsius per minute (° C./min), then heating the molded ceramic to a sintering temperature of 1,050° C.-1,150° C. with a heating rate of 2-4° C./min and then maintaining the sintering temperature of 1,050° C.-1,150° C. for 4-6 hours to obtain the ion-modified microwave dielectric ceramic with the chemical formula of Zn0.15Nb0.3[Ti1-x(W1/3Zr1/2)x]0.55O2.
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