CN111217603A - high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and preparation method thereof - Google Patents

high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and preparation method thereof Download PDF

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CN111217603A
CN111217603A CN202010083020.5A CN202010083020A CN111217603A CN 111217603 A CN111217603 A CN 111217603A CN 202010083020 A CN202010083020 A CN 202010083020A CN 111217603 A CN111217603 A CN 111217603A
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张平
杨苗苗
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Tianjin University
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Abstract

The invention belongs to the technical field of ceramic materials, and discloses a high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and a preparation method thereof, wherein the chemical formula of the material is Li2(Mg1‑xZnx)3Ti(O0.96F0.08)6X is more than or equal to 0.02 and less than or equal to 0.08; is prepared from Li2CO3、MgO、TiO2Proportioning LiF according to a proportion; carrying out primary ball milling, drying, sieving, and calcining at a certain temperature to obtain pre-sintered powder; the pre-sintered powder is dried, sieved, granulated, sieved and pressed into a green body after secondary ball milling; sintering the blank at a certain temperature, and cooling to room temperature after heat preservation to obtain the product. The invention adopts the traditional solid phase method and adopts F‑Ionic substitution of O2‑When the pre-sintering temperature and the sintering temperature of the lithium-magnesium-titanium ceramic are reduced by ions, Zn passes through2+Ionic substitution to increase Q f value of ceramics and produce low temperature sintered Li with high Q value2Mg3TiO6Is a microwave dielectric ceramic material.

Description

high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a ceramic composition characterized by components and a preparation method thereof, in particular to a high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and a preparation method thereof.
Background
With the rapid development of wireless communication technology, microwave dielectric ceramics attract more and more attention due to their specific functions and excellent characteristics in circuits. The microwave dielectric ceramic material has the advantages of low dielectric constant, low loss, high resonant frequency stability and the like, and is mainly used as microwave components such as resonators, filters, dielectric antennas, dielectric guided wave loops and the like in microwave circuits. The research on the novel microwave dielectric ceramic provides important material support for a microwave circuit.
In recent years, Li2Mg3TiO6The ceramic is a novel microwave dielectric ceramic system developed in recent years, has good microwave dielectric properties, but the research on low-temperature sintering is less. In previous studies, the addition of LiF after pre-firing only reduced the final sintering temperature of the samples, the pre-firing temperature of the ceramic was still higher. Due to F-Ions with O2-The ionic radii are similar and the F-ions are chemically stable at high temperatures compared to other anions, so that the addition of LiF to replace O by F-ions before presintering has been practiced by some researchers2The ions simultaneously reduce the pre-sintering temperature and the sintering temperature of the lithium magnesium titanium ceramic, but researches show that the quality factor Qxf value is greatly reduced although the pre-sintering temperature and the sintering temperature are effectively reduced. Therefore, it is necessary to research a low-temperature sintered lithium magnesium titanium ceramic material with a higher Q value.
Disclosure of Invention
To overcome Li2Mg3TiO6Microwave dielectric ceramic F-Ion pair O2-The invention provides a novel high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and a preparation method thereof, and aims to solve the technical problem that the Q multiplied by f is smaller due to reduction of pre-sintering temperature and sintering temperature through ion substitution, and Li is used for preparing the novel high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material2CO3，MgO，TiO2ZnO and LiF are used as main raw materials, and a traditional solid phase method is adopted to pass through F-Ionic substitution of O2-When the pre-sintering temperature and the sintering temperature of the lithium-magnesium-titanium ceramic are reduced by ions, Zn passes through2+Ionic substitution to increase Q f value of ceramics and produce low temperature sintered Li with high Q value2Mg3TiO6Is a microwave dielectric ceramic material.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a low-temp sintered Li-Mg-Ti dielectric material with high Q value is disclosed, whose chemical formula is Li2(Mg1-xZnx)3Ti(O0.96F0.08)6，0.02≤x≤0.08。
Further, x is 0.02, 0.04, 0.06, or 0.08.
Further, from Li2CO3，MgO，TiO2ZnO and LiF.
A preparation method of the high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material comprises the following steps:
(1) mixing Li2CO3，MgO，TiO2ZnO and LiF materials according to the formula Li2(Mg1-xZnx)3Ti(O0.96F0.08)6X is more than or equal to 0.02 and less than or equal to 0.08; carrying out primary ball milling on the obtained ingredients, deionized water and grinding balls for 4-8 hours on a ball mill according to the mass ratio of 3:18: 15;
(2) drying and sieving the mixed ingredients obtained in the step (1) to obtain mixed powder with uniform particles;
(3) calcining the mixed powder obtained in the step (2) at the temperature of 650-700 ℃ for 4-6 hours to obtain pre-sintered powder;
(4) performing secondary ball milling on the pre-sintered powder obtained in the step (3), deionized water and grinding balls for 6-8 hours on a ball mill according to the mass ratio of 3:18: 15;
(5) drying and sieving the powder obtained in the step (4), adding an adhesive for granulation, and pressing the powder into a green body after sieving;
(6) and (4) sintering the blank obtained in the step (5) at the temperature of 900-975 ℃, and preserving heat for 4-6 hours to obtain the high-Q-value low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic.
Further, the ball milling time in the step (1) was 8 hours.
Further, the calcination temperature in the step (3) was 700 ℃ and the calcination time was 4 hours.
Further, the ball milling time in the step (4) was 8 hours.
Further, the rotation speed of the ball mill in the step (1) and the rotation speed of the ball mill in the step (4) are both 250 r/min.
Further, the adhesive in the step (5) is paraffin wax, and accounts for 6-8 wt% of the dried and sieved powder obtained in the step (4).
The invention has the beneficial effects that:
the invention adopts different amounts of Zn2+Ion pair Li2Mg3Ti(O0.94F0.08)6Mg in ceramics2+Ion exchange, a certain amount of Zn2+The replacement of ions changes the crystal structure of the ceramic, causes lattice distortion and introduces point defects, promotes the sintering process, improves the density of the sample, and further effectively improves Li2Mg3Ti(O0.94F0.08)6The quality factor of the ceramic is that the raw materials are presintered at 650-700 ℃, and good dielectric property is obtained within the sintering temperature range of 900-975 ℃. Meanwhile, when 0.02mol of Zn is used2+Ion substituted Mg2+When ionic, efficiently convert Li2Mg3Ti(O0.94F0.08)6The Q multiplied by f value of the ceramic is improved to 128,000GHz, the dielectric constant is 14.64, and the temperature coefficient of the resonant frequency is-33.9 ppm/DEG C, so that the lithium magnesium titanium ceramic not only has lower pre-sintering temperature and sintering temperature, but also has higher Q multiplied by f value, and can be suitable for LTCC technology. In addition, the invention has simple preparation process, low raw material price and environment-friendly process, and is a microwave dielectric material with better application prospect.
Detailed Description
The invention is described in further detail below by means of specific examples:
the following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The invention adopts chemical raw material Li with purity more than 99 percent2CO3，MgO，TiO2ZnO and LiF are used to prepare novel high Q value low temperature sintering lithium magnesium titanium ceramics.
In the invention, Li2CO3，MgO，TiO2ZnO and LiF as raw materials and Li as chemical formula2(Mg1-xZnx)3Ti(O0.96F0.08)6(x is more than or equal to 0.02 and less than or equal to 0.08) mixing the following materials:adding deionized water and grinding balls into a polyester tank according to the proportion of 3:18:15, and carrying out ball milling for 4-8 hours; putting the ball-milled raw materials into an infrared drying oven for drying and sieving, and calcining for 4-6 hours at 650-700 ℃; putting the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, ball-milling for 6-8 hours, and drying; then granulating the dried and sieved ceramic powder with paraffin adhesive with the external weight percentage of 6-8%, and pressing the powder into a green body with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4MPa after sieving; sintering the green body at 900-975 ℃, and preserving heat for 4-6 hours to prepare novel high-Q-value low-temperature sintered lithium-magnesium-titanium ceramic; and finally, testing the microwave dielectric property of the product by a network analyzer and a related test fixture.
Example 1:
1. ceramic component Li according to microwave medium2(Mg0.98Zn0.02)3Ti(O0.96F0.08)6Term for Li2CO3-6.1972g、MgO-13.0764g、ZnO-0.5389g、TiO28.8135g, 30g of LiF-1.3740g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 4 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 650 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 6 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 900 ℃, and preserving heat for 4 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 2:
1. ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1415g、MgO-12.6944g、ZnO-1.0681g、TiO28.7343g, 30g of LiF-1.3617g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 7 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 900 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 3:
1. ceramic component Li according to microwave medium2(Mg0.94Zn0.06)3Ti(O0.96F0.08)6Term for Li2CO3-6.0869g、MgO-12.3192g、ZnO-1.5879g、TiO28.6565g, 30g of LiF-1.3495g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 6 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 7 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 6 percent of the powder by weight as an adhesive for granulation, and sieving by a sieve of 80 meshes; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 900 ℃, and preserving heat for 5 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 4:
1. ceramic component Li according to microwave medium2(Mg0.92Zn0.08)3Ti(O0.96F0.08)6Term for Li2CO3-6.0331g、MgO-11.9507g、ZnO-2.0985g、TiO28.5801g, 30g of LiF-1.3376g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder at 675 ℃ for 5 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 900 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 5
1. Ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1972g、MgO-13.0764g、ZnO-0.5389g、TiO28.8135g, 30g of LiF-1.3740g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 6 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 925 ℃ and preserving heat for 6 hours to prepare the low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 6:
1. ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1415g、MgO-12.6944g、ZnO-1.0681g、TiO28.7343g, 30g of LiF-1.3617g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 925 ℃ and preserving heat for 6 hours to prepare the low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 7:
1. ceramic component Li according to microwave medium2(Mg0.94Zn0.06)3Ti(O0.96F0.08)6Term for Li2CO3-6.0869g、MgO-12.3192g、ZnO-1.5879g、TiO28.6565g, 30g of LiF-1.3495g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 925 ℃ and preserving heat for 6 hours to prepare the low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 8:
1. ceramic component Li according to microwave medium2(Mg0.92Zn0.08)3Ti(O0.96F0.08)6Term for Li2CO3-6.0331g、MgO-11.9507g、ZnO-2.0985g、TiO28.5801g, 30g of LiF-1.3376g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 925 ℃ and preserving heat for 6 hours to prepare the low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 9:
1. ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1972g、MgO-13.0764g、ZnO-0.5389g、TiO28.8135g, 30g of LiF-1.3740g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 950 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 10:
1. ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1415g、MgO-12.6944g、ZnO-1.0681g、TiO28.7343g, 30g of LiF-1.3617g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 950 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 11:
1. ceramic component Li according to microwave medium2(Mg0.94Zn0.06)3Ti(O0.96F0.08)6Term for Li2CO3-6.0869g、MgO-12.3192g、ZnO-1.5879g、TiO28.6565g of-LiF-1.3495 g of complexTotal 30g of material; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 950 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 12:
1. ceramic component Li according to microwave medium2(Mg0.92Zn0.08)3Ti(O0.96F0.08)6Term for Li2CO3-6.0331g、MgO-11.9507g、ZnO-2.0985g、TiO28.5801g, 30g of LiF-1.3376g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 950 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 13:
1. ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1972g、MgO-13.0764g、ZnO-0.5389g、TiO28.8135g, 30g of LiF-1.3740g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 975 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 14:
1. ceramic component Li according to microwave medium2(Mg0.96Zn0.04)3Ti(O0.96F0.08)6Term for Li2CO3-6.1415g、MgO-12.6944g、ZnO-1.0681g、TiO28.7343g, 30g of LiF-1.3617g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and carrying out planetary typeBall-milling for 8 hours on a ball mill, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 975 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 15:
1. ceramic component Li according to microwave medium2(Mg0.94Zn0.06)3Ti(O0.96F0.08)6Term for Li2CO3-6.0869g、MgO-12.3192g、ZnO-1.5879g、TiO28.6565g of powder and 1.3495g of LiF powder are mixed, the mixed powder is added into a polyester tank, 180ml of deionized water and 150g of zirconium balls are added, and then ball milling is carried out on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 700 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 975 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
Example 16:
1. ceramic component Li according to microwave medium2(Mg0.92Zn0.08)3Ti(O0.96F0.08)6Term for Li2CO3-6.0331g、MgO-11.9507g、ZnO-2.0985g、TiO28.5801g, 30g of LiF-1.3376g of ingredients; adding the mixed powder into a polyester tank, adding 180ml of deionized water and 150g of zirconium balls, and then carrying out ball milling on a planetary ball mill for 8 hours, wherein the rotating speed of the ball mill is 250 r/min;
2. putting the ball-milled raw materials into a drying oven, drying in the drying oven and sieving by a 40-mesh sieve to obtain powder with uniform particles;
3. calcining the powder material at 750 ℃ for 4 hours;
4. placing the calcined powder, deionized water and zirconium balls into a polyester tank according to the mass ratio of 3:18:15, performing secondary ball milling for 8 hours, drying after discharging, and sieving by a 40-mesh sieve; then adding paraffin accounting for 8 percent of the powder by weight as an adhesive for granulation, and sieving by a 80-mesh sieve; pressing into a blank with the diameter of 10mm and the thickness of 5mm by a powder tablet press under the pressure of 4 MPa;
5. sintering the blank at 975 ℃, and preserving heat for 6 hours to prepare low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic;
and finally, testing the microwave characteristics of the obtained product by a network analyzer and a related test fixture.
The detection method of embodiments 1 to 20 of the present invention is as follows:
1. the diameter and thickness of the sample were measured using a micrometer.
2. The dielectric constant and the Qxf value of the prepared cylindrical ceramic material are respectively measured by an open cavity parallel plate method and a closed cavity method by an Agilent 8720ES network analyzer, the obtained ceramic is placed in a test fixture and placed in an ESPEC MC-710F type high-low temperature circulating incubator for measuring the temperature coefficient of resonance frequency, the temperature range is 25-85 ℃, and the test frequency range is 5-15 GHz.
TABLE 1 shows Li according to the invention2Mg3Ti(O1-x/2Fx)6(x is more than or equal to 0.06 and less than or equal to 0.12) relevant process parameters and microwave dielectric properties of various embodiments of the ceramic.
TABLE 1 microwave dielectric Properties
Figure BDA0002380965320000111
Figure BDA0002380965320000121
It can be seen from the above examples that the novel high-Q-value low-temperature sintered Li-Mg-Ti dielectric ceramic material studied in the invention2(Mg1-xZnx)3Ti(O0.96F0.08)6X is more than or equal to 0.02 and less than or equal to 0.08, which effectively improves Li2Mg3Ti(O0.96F0.08)6The quality factor of the ceramic is that the raw materials are presintered at 650-700 ℃, and good dielectric property is obtained within the sintering temperature range of 900-975 ℃. When x is 0.02 and the pre-firing temperature is 700 ℃, the ceramic is sintered at 950 ℃ for 6 hours (example 10), and the obtained ceramic has the most excellent properties: epsilonr～14.64,Q×f～128,000GHz，τf～-33.9ppm/℃。
Although the preferred embodiments of the present invention have been described, the present invention is not limited to the above-mentioned embodiments, which are only illustrative and not restrictive, and those skilled in the art can make various modifications without departing from the spirit and scope of the present invention, which falls within the protection scope of the present invention.

Claims (9)

1. The high Q value low temperature sintered lithium magnesium titanium series medium material is characterized in that the chemical formula is Li2(Mg1-xZnx)3Ti(O0.96F0.08)6，0.02≤x≤0.08。
2. The high-Q low-temperature sintered lithium-magnesium-titanium dielectric material as claimed in claim 1, wherein x is 0.02, 0.04, 0.06 or 0.08.
3. The high Q low temperature sintered lithium magnesium titanium based dielectric material as claimed in claim 1, wherein Li is selected from Li2CO3，MgO，TiO2ZnO and LiF.
4. A method for preparing the high-Q low-temperature sintered lithium-magnesium-titanium dielectric material according to any one of claims 1 to 3, which comprises the following steps:
(1) mixing Li2CO3，MgO，TiO2ZnO and LiF materials according to the formula Li2(Mg1-xZnx)3Ti(O0.96F0.08)6X is more than or equal to 0.02 and less than or equal to 0.08; carrying out primary ball milling on the obtained ingredients, deionized water and grinding balls for 4-8 hours on a ball mill according to the mass ratio of 3:18: 15;
(2) drying and sieving the mixed ingredients obtained in the step (1) to obtain mixed powder with uniform particles;
(3) calcining the mixed powder obtained in the step (2) at the temperature of 650-700 ℃ for 4-6 hours to obtain pre-sintered powder;
(4) performing secondary ball milling on the pre-sintered powder obtained in the step (3), deionized water and grinding balls for 6-8 hours on a ball mill according to the mass ratio of 3:18: 15;
(5) drying and sieving the powder obtained in the step (4), adding an adhesive for granulation, and pressing the powder into a green body after sieving;
(6) and (4) sintering the blank obtained in the step (5) at the temperature of 900-975 ℃, and preserving heat for 4-6 hours to obtain the high-Q-value low-temperature sintered lithium-magnesium-titanium microwave dielectric ceramic.
5. The method for preparing the high-Q-value low-temperature sintered lithium-magnesium-titanium-based dielectric material as claimed in claim 4, wherein the ball milling time in the step (1) is 8 hours.
6. The method for preparing the high-Q-value low-temperature sintered lithium-magnesium-titanium-based dielectric material as claimed in claim 4, wherein the calcination temperature in the step (3) is 700 ℃ and the calcination time is 4 hours.
7. The method for preparing the high-Q-value low-temperature sintered lithium-magnesium-titanium-based dielectric material as claimed in claim 4, wherein the ball milling time in the step (4) is 8 hours.
8. The method for preparing the high-Q-value low-temperature sintered lithium-magnesium-titanium-based dielectric material as claimed in claim 4, wherein the rotation speed of the ball mill in step (1) and the rotation speed of the ball mill in step (4) are both 250 rpm.
9. The method for preparing the lithium-magnesium-titanium dielectric material with the high Q value and the low temperature sintering function according to claim 4, wherein the binder in the step (5) is paraffin wax, and the mass ratio of the dried and sieved powder obtained in the step (4) is 6-8 wt%.
CN202010083020.5A 2020-02-07 2020-02-07 high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and preparation method thereof Pending CN111217603A (en)

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US20060214131A1 (en) * 2003-07-11 2006-09-28 Sang-Goo Lee Ferroelectric ceramic compound, a ferroelectric ceramic single crystal, and preparation processes thereof
CN102887701A (en) * 2012-09-24 2013-01-23 天津大学 Medium-temperature sintering low-loss microwave dielectric ceramics and preparation method thereof
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